How To Manufacture The D Enantiomer Of Phenylaminopropane And 3 4 Methyl Ene Dioxymeth Phenylaminopropane Essay

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Re: DETAILED METHODS for NON-CHEMISTS

METHamphetamine PRECURSS CLEANING/wkUP

Extractomania........by Ozbee friends..........edited by Placebo

INDEX:

1: Equipment

2: Ingredients

3: Method

step 1:

step 2:

step 3:

step 4:

step 5:

step 6:

4: Acid/Base

5: HCl-Gassing

6: Notes

1: Equipment

* Various jars, glass vessels, beakers etc

* PH paper, electronic PH tester

* Filter paper coffeee filters

* A strainer that will fit your filters nicely,

so that you get better surface area then a funnel

* Hair dryer, heat lamps

* Hot plate, no open flames, only heat elements

* Seperaty funnel, similar, tube to siphon

2: Ingredients

-Pills containing psuedo-ephedrine HCl ephedrine HCl.

-NaOH/Sodium Hydroxide/caustic soda/strong base/lye.

-Epsom salts that have been baked in oven 200c f an hour to dry.

-Methanol

-Acetone

-Toluene

-Distillated water

3: Method

***e*** :

If pills have red coating, put in jar, with acetone, shake until red coating is dissolved then continue as

below.

Step 1: First, put your pills in a jar.

Add methanol about double the volume of the pills.

Cap the jar shake till they break apart.

Leave to sit f a few hours shaking every 1/2 hour.

Let settle into 2 nice layers then siphon decant off top layer.

No need to get it all as we will do this 2 me times to be sure get all that pseudo.

step 2: Once you have done it 3 times have the 3 lots of methanol from above, put them together

put in freezer.

You want to get it real cold, near freezing then filter it thru a very fine filter, this may take some time if

you don't have a vacuum filtration setup but thats ok, we aint in a hurry.

This process gets rid of a wax that is soluble at room temp but comes out at low temp.

step 3:***e*** : This step is necessary only speeds things up.

After the chilled filter, we will reduce the volume of methanol/pseudo solution.

So, with good ventilation a fan blowing over pot, just reduce the volume of methanol, but till you

see crystals anything. Just reduce it to a manageable amount, we just want a saturated solution, you'll

ice it thicken a bit. Stop, take it off.

step 4: Now you want to pour a thin film of this methanol/psuedo solution out on a mirr glass table f

fast evapation, you could just leave it laying around a couple of days let nature take its course,

it does make pretty crystals. Scrape all your crystals up when they are dry put into aher clean pyrex

vessel.

step 5: Now pour Toluene, about double your psuedo volume **dry/anhydrous**use your epsoms!** over

your powdered psuedo, heat till just befe boiling with your fan blowing over it.

Boil f 5 mins then filter. Repeat this with fresh toluene until when you boil toluene it stays clear. To be

sure of toluene doing its job, after filtering, add water to toluene befe discarding you'll see the *censored*

come out.

step 6: Next you can do an acetone wash, by putting your psuedo some acetone in a jar, shake

filter. Dry pseudo you should have *censored*in clean pseudo HCl......

This procedure, rids the pills of:

MCC

waxes

polymers

lactose

most *censored*!

BUT, povidone! Me on that later.

You may choose to react your psuedo now.

Or do an A/B acid/base extraction, basicly turn it into a freebase, oil.

keep in mind..If you do an A/B now, you may lose some psuedo to the povidone.

So what are the choices? well, povidone is known to go thru Hi/RP, no problem, but must be steam distilled

out after. which is a good thing coz you got no seperations emulsions the cleanest meth around.

Povidone is bad because povidone is known to absb hold amines. It depends on what reaction your

doing!

4: A/B: Ok, get your nice dry white powder add about equal part water.

Now make up a 20% NaOH solution 4 parts DH2O:1 part NaOH.

Add Toluene to water/pseudo solution about equal to water volume.

Yes, toluene first, it gives the pseudo somewhere to go instead of being burned by the base which can break

it up turn it into aziradines!toxic!

Add NaOH solution to water/pseudo/toluene solution till PH 13, remember to test PH of water toluene!

Now shake the jar up very well let settle into layers.

Seperate toluene layer. Repeat this process 3 times combine all your toluene.

You can wash the toluene/pseudo freebase with water now, if you like, seperate again.

Now you can either, evapate toluene f freebase crystals, you need to turn the freebase into a Hcl salt

again.

So you can add fresh DH2O about 2mL f each gram of pseudo to your toluene drop HCl acid slowly

with shaking each time into the toluene. Check pH all the time stop just befe neutral. Shake again,

recheck, this is very tricky takes patience.

Now seperate the water from the toluene.

Now you can evapate your water to get your pure pseudo HCl.

You can repeat this aher 1 2 times get a little me.

5: Gassing,

Gassing makes things easier coz you just gas it, filter there'r your crystals, but it is tricky to get the

hang of it Hydrogen Chlide is dangerous! It will burn your *censored*in lungs instantly if inhaled too much of it!

You need to pipe HCl gas into your jar full of toluene pseudo freebase, but the gas your toluene must

be dry : no water, everytime the gas fms crystals it will be reabsbed by the miniscule amounts of

water.

If you don't know how to extract, you shouldn't play with gas yet.

If you know how to gas then read on...

So, you need to dry your toluene/pfed solution with pre-baked epsom salts to absb the water, then

filter them out. Then gas your solution you will see a snow stm befe your very eyes.

Then just filter dry crystals.

But still may contain povidone.

Post merely f infmational purposes. I haven't done anything illegal n should you.

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

METHamphetamine synthesis

I.----Placebo's compilation of "the Cure" by Ozbee clean-up of sudafed other ephedrine pills

various RP/I2red phosphous / elemental iodine, pure, crystals methods.

placebo

Hive Researcher

07-04-00 11:04

Go to whoah!

Ok, this is a compilation of many peoples' methods.

I believe this to be the best, simplest, fastest, cleanest method f producing meth-amphetamine,

in the highest yields possible f RP/I2/E reaction.

Remember, each every step gives small losses, this method has the least steps!

It is a culmination of effts by wlock, CHEMMAN, maybe a few tiny touches by me.

I re-iterate, I don't want any congratulations except f the write-up itself.

You will need these things, no substitutions allowed.

If you can't get this *censored*, you ain't ready to make the best Go-Go in town.

This is a refinement of all methods, the next step up from Push Pull, but nobody should be discouraged

from attempting this, as you will probably find it easier.

pH paper isn't even necessary.

This post is one method from Go to whoah.

This post has to be followed from Go to whoah.

Otherwise you can run into trouble, as povidone is removed in this extraction.

It will be removed at the end. Each step was chosen to complement the next.

Underst?

Read on.....

Index:

1: Equipment

2: Reagents

3: Extraction of pfed

4: Reaction

5: Steam distillation

6: Crystallisation

Equipment:

Various jars

2L pyrex vessel

2L 2 neck round flat bottom flask

1 condenser, I recommend a coil condenser but a Liebig will suffice.

1 sloping splashhead better, a steam distillation sloping splashhead.

A steam pressure cooker, that has a release-valve on top.

Hotplate, electric of course.

Filter paper, Buchner vacuum would be nice too.

Thermometer.

1 Glass stopper.

Lengths of clear pvc tubing.

Pot with vegetable oil, which can fit your reaction vessel.

Reagents:

Iodine crystals.

Red Phosphous.

Pseudo-ephedrine, ephedrine.

Methanol.

Toluene.

Acetone.

NaOH.

All must be clean anhydrous.

Ice.

Extraction of pfed:

This method will deal with the HCl salt of pfed, a streamlined version of "the Cure".

All pills are dumped into a large jar double of this pills-volume in the fm of methanol poured on top.

This is stirred vigourously let st to settle thereafter, in the fridge seems to speed it up.

After the top methanol layer has cleared it is carefully decanted off.

This procedure is repeated 3 times.

All methanol pulls are put together the methanol boiled off on a hotplate.

As methanol gets down to the last little bit, it is taken off the heat.

Then a ption of acetone, twice your remaining liquid is dropped in.

This fces the pfed crystals to crash out.

Then the remaining liquid is carefully evaped off.

washes:

Now you have your crude/dirty pfed HCl.

Next we will be doing successive toluene washes.

Put your pfed crystals in a pyrex heat proof glass.

Now add toluene to a safe level that can be lightly boiled on the hotplate.

After about 5 mins boiling with stirring, take off the heat let it settle a minute.

Now carefully pour off toluene into a filter to catch any remnants of pfed that may follow.

Now if you get the toluene that has our contaminants in it add some water, you will see the crap, crash

from the toluene into the water.

This is the crap that came thru with the methanol pull.

So as we continue to do multiple toluene washes, we will continue to test the toluene after pouring it off, to

see how we are progressing with the cleanup.

when we have reached a point where no crap comes out of the toluene, with the addition of water, then we

are ready to try acetone.

Usually about 3 boils in toluene, but of course it depends how much you'r using.

So, as befe we will add a ption of acetone boil lightly.

Now when we pour off the acetone, we will add a tiny amount of water some NaOH.

This is our final test, when you do this no crap falls out of acetone you are ready.

This will be the cleanest pfed you have ever seen, guarenteed!

, yields should be *90% if you'r carefull! 95% is good.

Reaction :

Smallest reaction to be attempted, especially by newbees, is 1 oz of pfed, so that even taking into account

sloppiness, lack of experience losses along the way, you should get some product.

Ratios of reagents are: 3:3:1 1:1:1/3 , ie.E:I:RP aka, equal amounts of Iodine pfed, a one third

amount of RP.

This is calculated on a weight basis, can be scaled up down as necessary, e.g.60gmE/60gmI2/20gmRP

120gmE/120gmI2/40gmRP etc etc.

First prepare yourself an icebath. Yes, icecubes water in a sink bucket.

Now, many will say you should add this first that first.

well, after much reading of different peoples methods, I say....

Chuck the whole shebang in together, while your flask is on ice, lift swirl ingredients together, while

maintaing on ice.

Put your condenser on top start water running thru, from bottom to top.

Now, the idea is to get the reaction going in the most controlled way possible, you want to let the reagents

react in the container vessel fixed in the icebath, if at all.

Then move vessel from icebath to room temp.

If things look like they're going too fast, put back in ice bath, you want to keep the reaction going but only

at a nice slow, controlled pace.

This is also necessary to control vapour in the condenser!

Thick dis-coled smoke is bad, plumes of smoke will escape from condenser.

Let things progress at a nice slow pace, as things slow too much, you can start applying heat.

So prepare an oilbath bring to about 50 C, if there is no me action in your vessel.

You can move it to the oilbath, the same goes f it as befe, when things slow down.

Adjust heat up, to say 100 C then 150 C f one hour, to make sure reaction has completed.

The whole time you should be watching to keep a nice reflux going, too much vapour is escaping

from condenser.

Now remove from heat disconnect condenser, add ice water to quench reaction.

The reason f ice water is to calm the reaction down when NaOH is added.

Its up to you if you want to filter out RP leave it in untill the end.

I would leave it, it will be washed nicely by next process be easier to filter.

Now add lots of NaOH to bring reaction mix to + 14 pH.

You can over-basify, as meth won't be destroyed, its a tough MF!

Steam Distillation :

Now you need to set up your glassware f steam distillation.

Attach the steam distillation sloping splashhead to top hole of flask, attach plastic hose to steam inlet

the other end on the release valve of the pressure cooker that is full of water.

Attach condenser on the end of splashhead, rig the whole up so it stays up.

Place a jar at the end of condenser to catch our distillate.

You want to heat both the pressure cooker, the reaction flask.

Sit back get ready f one of the most beautiful sights smells.

The meth freebase that is sitting on the top of your aquaeous layer in the flask will vapourise be carried

across be condensed in the condenser trickle down into your jar. It will sit atop of a bottom layer of

water.

After the last of the oil has come across, change jars leave the setup to run f aher hour, just to

make sure you got it all.

Any povidone from the pills will be stick behind in the reaction vessel.

It has been ed that some polymer that may have been left from extraction, may follow the steam.

Crystallisation :

Now we have a jar of water, with this sweet clear oil sitting on top.

Next options are to add HCl acid slowly with stirring until the oil layer disappears, then evap the whole lot

to get crystals.

Or, as I found, you may have some polymer that has come over with the steam, is now sitting in the

water layer, it looks cloudy.

I don't want to evap all that, it will just concentrate the *censored* in there, plus its very time consuming evapping

water, plus you risk losing some meth as the water evaps.

I think you should just throw a little toluene into the jar,

then seperate.

Now your absolutly pure meth freebase is in your toluene!

Now you can either gas, f instant the now clean meth,

add minimal distillated H2O then acidify to pH 7, shake, seperate evap water f crystals.

Repeat this step if you do it this way, as some me may come in a second go.

with this process from start to finish, you shouldn't need to re-crystalize, as your product should be the

cleanest *censored* anybody has ever seen anyway.

But you may want to, f the purpose of growing nice big crystals.

In which case, add just enough hot methanol to dissolve all your meth then place in freezer.

The secret is, the slower the evap, the bigger the crystals.

So a nice slow room temp evap over several days might be fun.

Enjoy, do attempt anything above, befe you completely underst what you are doing!

You must have a sound understing of the basics first!

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

--------------------------------------------------------------------------------------------------

How to produce anhydrous = dry = waterfree! HCl gas using no special equipment f all your

amination steps of freebases - by Psychokitty.

--------------------------------------------------------------------------------------------------

To date I have never used Strike's Fester's method f producing HCl gas.

Reasons f this are as follows:

1. The necessity of labaty glassware no OTC hardware.

2. what seems to be a messy proceedure using table salt but I wouldn't know

exactly as I've never tried it.

3. Difficult dismantling process at least it seems to be me difficult than

mine.

I don't remember the exact journal reference that inspired my method, but I do

know that it is described somewhere in Inganic Syntheses Vol. I.

Okay. First, here is what you need:

1. Beer bottle transparant.

2. Plastic baby syringe 15 ml capacity found at the pharmacy section at any

grocery ste.

3. Four so feet of ice-maker transparant-white polyethylene tubing found at

the hardware ste. I don't remember the exact diameter size. All I know is

that it IS the smallest size available.

4. One table-leg stopper rubber, beige black. Aher item of which I don't

know the size. Just take your beer bottle into the hardware ste see

which size fits snuggly on its top.

5. One aluminum tube that is the exact diameter size as the polyethylene tubing.

Found at the hardware ste but don't know what they are used f. They are

sometimes made of brass.

6. One bottle of sulfuric acid drain cleaner.

7. One bottle of concentrated hardware ste muriatic acid 32%?

Assembling the HCl generat is easy.

1. Use the aluminum tubing to burrow two holes to the top of the table-leg

stopper. Use a twisting motion while appling pressure f about a minute

eventually the tube will pop through.

2. Place the table-top stopper over the top of the beer bottle. It'll fit snugly.

3. Insert the polyethylene tubing into the middle-most hole push through

until the tubing hits the bottom of the beer bottle. with scisss a knife

cut off the polyethylene tubing about two inches from the top of the beer

bottle.

4. Take the entire table-top stopper inserted with the polyethylene tubing off

of the beer bottle. Pour into the beer bottle a volume of sulfuric acid about

an inch high off of the bottom of the beer bottle.

5. Replace the table-top stopper/polyethylene tubing on top of the beer bottle.

Insert the remaining tubing into the last hole of the stopper until about

two inches into the bottle. Cut tubing down to desired length.

6. Pour about twenty milliliters of concentrated HCl into a cup. Extract into

baby syringe until syringe is full 15 mL. NO, the HCl will dissolve

any part of the syringe in any way.

NEITHER THE HCl N THE SULFURIC ACID wILL REACT wITH ANY PIECE OF HARDwARE USED

IN THIS SYSTEM. THIS SET-UP HAS BEEN TESTED MANY TIMES wITH SUCCESS.

7. Insert the syringe into the middle tubing the one that extends to the bottom

of the beer bottle. End should be submerged in Sulfuric acid. If insertion

is difficult, use a knife to scrape the inside of the tubing to allow the

syringe to fit me easily.

8. Securing the set-up with a clamp of some st attached to a st is optional

but desirable.

9. Have hy on the side a container full of water.

The use of this set-up to gas ones solvent/amine is just as easy.

1. with right h, hold the tubing that will expel gas lower into the

solvent/amine solution.

2. with left h slowly start to inject the HCl solution in the syringe into

the sulfuric acid. Once it hits the acid, there will be alot of fizzing

foaming IMMEDIATELY HCl gas will be pumped into the solvent/amine solution.

Foaming is sometimes a problem as it starts to reach the top of the beer

bottle. Simple wait a while let it settle then continue. Sometimes

certain brs of drain opener can cause excessive foaming. If this occurs,

switch brs.

3. One syringe is usually enough f an amount of about 30-40 g of product, but

if me is needed after all the HCl has been injected, slowly SLOwLY remove

the syringe from the tubing, first be letting a crack of air into the system.

BEwARE that this is suddenly going to bring a min rush of HCl from the gassing

tube so make sure that it is submerged when doing this step. To continue, refill

the syringe proceed as described above.

4. Once the gassing is complete, leave the syringe ATTACHED to the injection

tube submerge the gassing tube in the container full of water If the

syringe is attached to the injecting tube, the following sequence will

occur. weigh down the gassing tube somehow as it must remain submerged.

In a few minutes about five the sulfuric acid will cool a bit causing a

sucking-back of the water into the beer-bottle. This will happen very suddenly

very fast, but to wry as the water will only go in as far as the top

of the beer bottle. This is actually an advantage as in this way one is able

to dilute the remaining HCl gas the remaining sulfuric acid. Of course the

bottle will get hot but if left aside f a few minutes it will eventually

cool making opening the container dispensing with the acid solution an easy

task. If the bottle is opened f whatever reason without the above acid

dilution step, HCl gas will be everywhere.

Hope this method will prove useful to you my fellow bees, it sure has been f me!

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

wISDOMwillwIN

Re: DETAILED METHODS for NON-CHEMISTS

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

Methyl_Man (Hive Researcher) 06-05-00 10:40 :

METHYL_MAN's WRITEUPS of MeOH BENZO WACKER and MeNO2-Al-Hg.

Consult these threads to avoid unnecessairy questions :

http://rhodium.lycaeum.org/clandestine/gonzo/index.html

/perl/showflat.pl?Cat=&Board=methods&Number=13991&page=

&view=&sb=&vc=1" target=_newhttp://hive.lycaeum.org/wwwthreads/perl/showflat.pl?Cat=&Board=methods&Number=13991&page=

&view=&sb=&vc=1 and

/perl/showflat.pl?Cat=&Board=methods&Number=15667&page=

0&view=collapsed&sb=5" target=_newhttp://hive.lycaeum.org/wwwthreads/perl/showflat.pl?Cat=&Board=methods&Number=15667&page=

0&view=collapsed&sb=5 and

/perl/showflat.pl?Cat=&Board=methods&Number=31473&page=

0&view=collapsed&sb=5" target=_newhttp://hive.lycaeum.org/wwwthreads/perl/showflat.pl?Cat=&Board=methods&Number=31473&page=

0&view=collapsed&sb=5

---------------------------------------------------------------------------------------------------

Here they are, with minor changes from older versions for greater accuracy.

=================================================================================

Methyl Man's MeOH version of the benzoquinone wacker

Materials:

400mL MeOH (methanol)

50mL distilled H2O

150g p-Benzoquinone

2g palladium (II) chloride (PdCl2)

178g safrole

DCM (methylene chloride; dichloromethane)

NaCl (non-iodized table salt)

Sodium bicarbonate (baking soda)

5% NaOH

HCl (hydrochloric acid, from muriatic acid)

Magnesium sulfate drying agent (epsom salts baked in 400¢XF oven for 2 hours)

Method:

1. In a 2L flask fitted with a reflux condenser and addition funnel place 400ml MeOH, 50ml dH2O,

150g p-Benzoquinone and 2g PdCl2 and leave to stir for a minimum of 60 minutes. Note that a recent

improvement has been discussed which involves stirring the PdCl2 in the solvent (MeOH in this case) for

several hours before adding the water and benzoquinone. It is likely that this does enhance yields a bit by

ensuring maximum efficiency of the PdCl2¡¦s catalytic action. Either way will work well, however. If you let

the PdCl2 stir alone for a while, when you then add the water and benzoquinone, let them stir for an hour as

well before beginning the next step so as to ensure complete dissolution of the benzoquinone.

2. Place 178g safrole mixed with a bit of MeOH in an addition funnel.

3. Add safrole dropwise from the addition funnel over 60 minutes or more. However, when the addition is

about 80% finished, apply low heat just sufficient to start a mild reflux (cold water through the condenser).

4. After the safrole addition is complete, leave mixture stirring and refluxing for 8 hours. (If you must stop at

this point and resume another day, be sure to put the mixture in the freezer, sealed well. The raw ketone

decomposes unless stored at freezer temperatures.)

5. Filter out the solids present in the mixture, which are hydroquinone (the degradation product of the

benzoquinone) and PdCl2. This can be done by vacuum filtration or by simple gravity filtration with coffee

filters. Many prefer gravity filtration with this synthesis because the solids produced in this reaction are very

fine and are problematic to filter with vacuum. Don¡¦t try to recycle the PdCl2, as it is too difficult to

separate from the hydroquinone to be worthwhile.

6. Flood mixture with 1.7L 3N (~10%) HCl. (Here's the quick math: add 500mL of 31% HCl [muriatic acid] to

1150mL H2O to get 1.65L ~10% HCl¡Xclose enough for this purpose.)

7. Extract flooded mixture with 3 portions of DCM (1 x 500mL, 1 x 250mL, 1 x 100mL) in a large separatory

funnel. The desired raw product, MDP-2-P (¡§ketone¡¨), migrates into the DCM as an oil. Separate the

DCM/ketone layers and combine them.

(Note: when you first hit it with the DCM you will probably observe a bit of scum which will float on top of

the water layer, which will work its way down during these three extractions to appear as a blob of spongy

semi-solid interface. It¡¦s actually very mobile and easy to work around; simply avoid allowing it into your

DCM separations. The same thing will happen in your washes in steps 10, 11 and 12 below, but by then you

will be quite the pro at working with it.)

8. Extract water layer with a final small amount of DCM.

9. Add this final small DCM extraction to the combined oil/DCM solution from step 8.

10. Wash the ketone/DCM solution with saturated sodium bicarbonate in water twice (500mL each wash).

11. Wash the ketone/DCM solution with saturated NaCl 3 times (400-500mL each wash).

(Note: as you do these bicarb and salt water washes, you should be seeing the ketone/DCM solution getting

progressively more greenish colored; this is visible in the film of solution that runs down the inner surface of

the sep funnel).

12. Wash the ketone/DCM solution 3 times with 500mL 5% NaOH (500mL each wash). If you did step 5, you

will have a very easy separation.

(Note: you should also see a very noticeable color change upon doing the first of these three washes wherein

the ketone/DCM layer becomes a strange, thick reddish-brown, almost orange color. This happens as the

NaOH pulls the majority of the solvated hydroquinone into its layer, cleaning the ketone. The NaOH layer in

the first wash will be very dark brown, almost black in fact. The next two will be a far lighter, watery, orangy

color.)

13. Dry the ketone/DCM solution with ~50g magnesium sulfate.

14. Distill off the DCM using mild heat on a water bath and ice-cold water through the condenser. This will

take several hours.

15. Add 50mL of high-oleic safflower oil (no additives!!) to the ketone oil as a buffer to prevent the ketone

from scorching in the distilling flask.

16. Vacuum distill the ketone/buffer oil mixture. This also will take a few hours, but not as long as distilling

the DCM off did.

17. At 100 to 140¢XC (wherever your particular vacuum dictates), a minor amount of safrole might come over.

If your safrole-to-ketone conversion was good, there should only be a very small amount. If it is only a few

drops to a milliliter or two, you can leave it in, and not change/clean receiving flasks. If you are a stickler for

purity, discard it. It will not harm anything later if you leave it in. But if it¡¦s more than a couple of milliliters,

get rid of it.

18. At anywhere from 25 to 40¢XC above the temperature your safrole usually comes over with the same

vacuum, the ketone should begin coming over. You should get about 100 to 120g ketone. The color of the

ketone coming over will likely be a pale, fluorescent-looking greenish yellow. In fact it looks not unlike

anti-freeze¡Xa similar ¡§neon green.¡¨ You can stop distilling when the rate of ketone coming over has slowed

to an agonizing one drop per 90 seconds or so. At this point there is so little left that it is probably not worth

your time to wait for a drop per 1.5 minutes (it¡¦s not worth mine anyway).

19. Immediately store your precious fluid in the freezer in an airtight sealed flask or bottle. Happy cooking!

---------------------------------------------------------------------------------------------------------

The MeNO2-Al-Hg reductive amination according to Methyl Man

Since the appearance of Ritter's writeup of this method in Total Synthesis II, much discussion has taken place

about it but, it has sometimes seemed, little has been clarified. This is due in large measure to the sensitivity

of this reaction to even the most minor changes in its many variables. With this writeup, I hope to provide a

clearer view of the method and to allow others to benefit from the hard-won experience of someone (not me)

whom we'll call Mr. A. Ritter's original writeup, while inspiring, lacked details about the many nuances that,

once understood, allow the amateur chemist to really understand this reaction's dynamics. Thus I have tried

with this writeup to help the neophyte who has only physical observations and scant written material to guide

him (although I suspect and hope that it may even help a few more seasoned cooks as well).

The first thing I'd like you to look at is the array of interrelating variables in this reaction that make it so

delicate. They are as follows:

1) the thickness/type of the aluminum

2) the consistency (i.e. flat, ground, etc.)

3) the amount of HgCl2 used in relation to the amount of aluminum

4) the addition rate of the MeNO2/MDP-2-P

5) the size of the reaction vessel in relation to the scale of the reaction

6) the ability to effectively stir the reaction

7) the coldness of the water through the reflux condenser (yes, even that!)

The above factors are sort of submitted in an order of importance (#1 being most important), but in reality

they are all inextricably related. I observed firsthand the trials and tribulations of Mr. A as he struggled to

match up the correct combination of ratios and conditions that would allow a smooth, consistent reaction

and predictable results every time. Finally, after lots of frustration, confusion, losses, and---in the end---a

revelation, the perfect set of elements was hit upon and recorded.

The scale Mr. A chooses to perform this reaction on is half-scale to the scale in the Ritter writeup, which was

55g aluminum and 50g MDP-2-P. Therefore this writeup will illustrate the reaction on a scale of 27.5g aluminum

and 25g MDP-2-P. The subject found for his own personal reasons that this smaller scale was much easier to

manage (not the least of which is that even with a huge 4-liter separatory funnel, at this smaller scale it gets

pretty filled up!). There's no doubt that the original larger scale can be successfully applied, although it would r

require adjustments in the glassware capacity, stirring method, and probably other elements.

MATERIALS and APPARATUS:

-- 27.5g Reynolds Wrap Heavy Duty aluminum foil

-- 25g MDP-2-P

-- 20 mL MeNO2 of 99+% purity

--750 mL MeOH + 50 mL more for addition funnel + additional small amounts that will be needed later to thin

the mixture

--400mg HgCl2

-- 2-liter 2-neck flat bottom flask

-- reflux condenser (400mm preferable)

--250mL or 500mL addition or separatory funnel

-- cooling setup (bucket, water pump, tubing, 1 large bag ice)

METHOD:

1. Weigh 27.5g of Reynolds Wrap Heavy Duty aluminum foil (NOTE: it HAS to be Reynolds and it MUST be the

heavy duty stuff) and then tear it by hand or cut it with scissors into small rectangles approximately 1" by

.75". Settle down with this task with a good CD or TV show because it is tedious and may take about

1.5 to 2 hours.

2. With a coffee grinder, "grind" these pieces of foil for durations of about 10 seconds. Fill the coffee grinder

only loosely (about two thirds full---don't stuff it! That will adversely change the consistency of the

ground foil). It will probably take about 4 to 5 "loads" in your grinder to do the whole amount of foil,

depending on the size of your grinder. (In actuality, the foil does not get "ground," but rather, each

individual piece just gets compacted and compressed. If it is compressed too heavily, the inner surfaces

of the foil nuggets may be rendered inaccessible to the Hg/MeOH solution, changing the timing of the

amalgamation and maybe even causing an incomplete or failed reaction.) When properly done, the foil

should be in gnarled little nuggets about the size of long-grain rice grains and should look really tight and

small. The smaller, the better for good stirring.

3. Place a 3" stirbar in your 2L flat bottom flask and onto your stirplate. Add the foil nuggets to the flask and

then proceed to set up your glass, support and clamps so that the reflux condenser and addition/sep

funnel are securely affixed and your flask is well-centered on the stirplate (this will be critical when you

begin to attempt stirring!). Also, prepare your cooling, i.e. attach the inflow and outflow tubes to the reflux

condenser.

4. Carefully add the 400mg HgCl2 to 750mL MeOH to a tightly sealable bottle and shake to dissolve all HgCl2.

Set this solution aside.

5. Combine the 25g MDP-2-P, 20mL MeNO2, and 50mL MeOH and pour them into the addition/sep funnel.

Rinse your beaker (or whatever you used) with a tiny bit of additional MeOH to get the residual ketone and

add it to this MDP-2-P/MeNO2/MeOH solution.

6. Very slowly and carefully (w/gloves, glasses, long sleeves and a Hail Mary if you're Catholic), using a large

funnel, pour the HgCl2/MeOH solution from step 4 down the condenser.

7. Turn the stirring on full blast for a 5-second burst to intimately mix the solution and the foil. If you...

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