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[*] posted on 8-4-2011 at 06:13
a digression about N-methylalanine


I am trying to find a way to get formaldehyde to make N-methylalanine. I can make formaldehyde by adding Hcl to hexamine and it then forms a solution of formaldehyde, water and ammonium chloride. I can then use this solution to react with the zinc and alanine to make the n-methylalanine. But When the crystals of N-methylalanine form overnight there is much ammonium chloride present in the crystals and it must come out.
Therefore I was thinking that if I crush the crystals up into a fine powder and then shake it with water several times and then filter off the fine N-methylalanine powder into a coffee filter that maybe all the ammonium chloride will be dissolved into the water and therfore this is how I can extract the ammonium chloride from the N-methylalanine fine powder.

Does anyone have any opinions about this procedure that I have just described?
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[*] posted on 8-4-2011 at 20:04


my opionion, kewl man!!!!
but if you knew anything about chemistry there is this thing called the gigo principle.
garbage in, garbage out.
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[*] posted on 8-4-2011 at 22:57
n methylalanine


That would be right somone without a lot of knowledge asked a question about n methylalanine and they get treated like they are a drug cook. It makes me sick some of the people on this site after all there is no proof that that is the case at all.
If these people know of these procedures you have to ask your self what there motivation is . further more no wonder this site has lost a lot of good people.
I don't see anything in this post that mentioned amphetamines or any pecurser to amphetamines.
There has been to much of this shit going on for a long time it is about time the moderators stood up and got rit of these people.
In the real world of law the people would be charged with defermation but they would rather hide behind there computer.

By the way you could seperate the n methylalanine by recrystalising it from ethanol as ammonium chloride is not soluable in it.

bullshit bullshit bullshit

REGARDS AZO



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[*] posted on 9-4-2011 at 00:30


Thanks Azo I appreciate your support.
Could you please tell me the whole process you believe that I could do to get the ammonium chloride out of the N-methylalanine crystals?
(assuming I have already got the n-methylalanine crystals and the ammonium chlorde is still in it)

cheers mate
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[*] posted on 9-4-2011 at 02:57
n methylalanine


I don't no the solubility of the amino acid but because it has a amino group and a carboxyl group it would be soluable in ethanol or at least when heated then filter out the ammonium chloride and evaporate down the alcohol to get your amino acid.
you would also need to consider seperating out the over alkylated amino acid and other impurities.
! unless you have a way of acheiving monoalkylation if so me and a lot of others would like to here it.


regards azo

i think solo was playing with this at some time maybe ask him to.
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[*] posted on 9-4-2011 at 13:59


defamation man that's rich!!! i love it
but you said defermation.
last time i checked that is'nt even a word in the english language.
so if you were to serve me for defermation i would say the complaint is invalid on it's face.

personally i don't care if your making drugs, but at least do some homework before asking questions.

[Edited on 9-4-2011 by jon]

[Edited on 9-4-2011 by jon]

[Edited on 9-4-2011 by jon]
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[*] posted on 9-4-2011 at 14:45


defamation , if only they would get rid of them. Defamation of someone, spoken out loaud and in a public place with witnesses, will stand up in a court of law. I see no reason why the keyboard typed word should be exempt from the same law. even if deleated, there is still a record of it being typed up, & from which ip address it was from, let's not go there, we would be no better then them if we travelled that road.
theres mono methylation on rhodium,s site. also, can UREA be used to help solubility & help minimise unwanted side reactions? or is this somthing I have read about another rxn and has no bearing on this one? it wouldn't be the first time. lol

IIRC, camper toilet fluid (blue) is formaldehyde, or get some from a biology site, I use it to store unusual looking or unidentifyable dead bugs whilst gardening.


To get the ammonium chloride out of the methylamine, it is reduced by heat and cooled to crash out the ammoniam chloride, I have no idea if this aplies to all methylamine recapies.

hope these helped. Xtal
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[*] posted on 9-4-2011 at 14:55


it's much harder to bring a defamation case than you think.
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[*] posted on 9-4-2011 at 15:30


When did that happen? not that long ago, I was with a friend who had a small group aproach him, and one of the group happened to anounce (rather loudley) a debt of money that was owed to him, then a small scuffle ensued.
When he was talking to a solicitor about it, he said a debt becomes null & void when the ammount is publicly anounced or demanded, also to be carefull of what he say's to him or about him publicly, as def of charic comes into play. Admittidly, he didn't say it would be easy or hard, only that it was something to be aware of.
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[*] posted on 9-4-2011 at 15:39


good and well it depends a lot on the circumstances.
since an opionion was asked and an opionion was given; permission was granted to state an opionion.
defense #1

since the claimaint is operating under a psuedonym the claimaint has no real world reputation at stake therfore, no damages can be assessed in this matter.
defense # 2

no actual defamation occured since the opionion rendered did not state implicitly or explicitly, that the claimaint was engaged in criminal activity

defense #3 shall i continue?

[Edited on 9-4-2011 by jon]
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[*] posted on 9-4-2011 at 16:39


I will have to continue this via u2u, delicate situation
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[*] posted on 9-4-2011 at 18:00


i saved the best defense for last

plantiff is incapable of further defamation–e.g., the claimant's position in the community is so poor that defamation could not do further damage to the plaintiff. Such a claimant could be said to be "libel-proof", since in most jurisdictions, actual damage is an essential element for a libel claim. Essentially, the defense is that the person had such a bad reputation before the libel, that no further damage could possibly have been caused by the making of the statement.
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[*] posted on 10-4-2011 at 01:16
n-methylalanine


you mean to tell me that when Imake the N-methylalanine, I'm also making over alkylated amino acids also?
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[*] posted on 10-4-2011 at 01:59


Yes. amino acid not amino acids

[Edited on 10-4-2011 by azo]
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[*] posted on 10-4-2011 at 03:29
n-methylalanine


what if I was to make the N-methylalanine (with the ammonium chloride inside it) and then crush the n-methylalanine crystals to a fine powder and then shake it with water and then filter off the N-methylalanine by pouring the solution through a coffee filter.
I'm guessing that the water will absorb all the ammonium chloried particles out and the n-methylalanine powder will be left in the coffe filter.
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[*] posted on 10-4-2011 at 04:22


If you read my prior post you will see that the amino acid is soluble in ethanol ! which means the amino acid would also be soluble in water , how are you going to seperate it then ,

regards azo
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[*] posted on 10-4-2011 at 04:35


are we talking b-alanine d-alanine l-alanine or dl-alanine to N-methyl-?-alanine?
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[*] posted on 10-4-2011 at 05:02
n-methylalanine


we are talking about L-alanine to N-methylalanine
and N-methylalanine is only slightly soluble in water, I've tried it.
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[*] posted on 10-4-2011 at 09:11
CLEAN UP


SORRY, I should have said toluene by all acounts. followed by washing and salting.
It a speciality chemical compound, and there seems to be little in the way of info out there.
I did however, come across this.
chapter 18 is what your after, I believe this will have enough info on the solvents,methods used to clean it up and salt it out.
..LET THE FLAMEING BEGIN.......drum roll Xtal:D
ok, the pdf book is 9mb in size, so I can email you the book, or let me know how to resize it. X



I would say DMSO, there seems to be verry little in the way of properties, solubilities available. The only info I have mentions DMSO, along with more productive methods of manufacture.

[Edited on 10-4-2011 by crystalXclear]

[Edited on 10-4-2011 by crystalXclear]
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[*] posted on 10-4-2011 at 16:37


at last,thank the elemental spirits for digital editing.
This is the only usefull info on this reaction I can find at presant.

Chapter Eighteen
Cooking Your Own Ephedrine
You don't like that recipe? Check out this one taken from "Chemical Abstracts ", Volume 47, column
3347. Twenty grams of N-methyl-d,l-alanine and 50 grams of benzaldehyde are placed in a flask and
heated on an oil bath at 1 50- 1 60° C until the mixture stops fizzing otT carbon dioxide.
The mixture is then cooled and mixed with a few hundred ml of toluene. Whatever doesn't dissolve
in the toluene is thrown away. The product, which is a mixture of ephedrine and pseudoephedrine, is then
extracted out of the toluene by shaking the toluene with about an equal volume of 1 0% HCI. The toluene
can be distilled to recover unused benzaldehyde, if there is any in it.
The dilute hydrochloric acid solution which contains the products should be boiled down to
concentrate it. The steam will also carry off some byproducts, so vent this steam outside.
Once the dilute acid has boiled down to a volume of 50-100 ml, allow it to cool. Then add a little
activated carbon, and stir it around for a while. Then filter it out. This will decolorize the solution.
Add lye pellets a little bit at a time with stirring until the water solution is strongly alkaline. Extract the
alkaline water a few times with toluene. The combined toluene extracts should next be bubbled with dry
HCl gas to give a crystalline product amounting to about 1 2 grams. The product will be about 8 grams of
d,l-pseudoephedrine, and 4 grams of d,l-ephedrine. lt will yield racemic meth upon reduction.
Take note that recovering ephedrine from water solutions is a bit different than recovering meth.
That's because ephedrine free base dissolves well in water, while meth doesn't. So for recovery of the
ephedrine we take the dilute acid solution of the ephedrine and boil it down, j ust like in the pill extraction
procedure using waler. Once it is concentrated, then it is made alkaline with lye, and lhe ephedrine
extracted out. In this way you get good recovery of the ephedrine. Use too much water, and it's difficult
to extract it all out.
This original recipe seemed good on the face of it, but it suffered from serious problems. The yield of
product was low, as a lot of tar was made in the reaction. The starting material, N-methyl alanine, is not
commercially available at a reasonable price, and it used to be not easily made by the methods available
then.
These problems have been conquered by advances made with the passage of time. The large amount of
tar made in the reaction is prevented if DMSO is used as a solvent in the reaction. DMSO also allows the
temperature of the reaction to be lowered to 1 20 to 1 30 C. DMSO, or dimethylsulfoxide, has found wide
use as a pain reliever for creaky joints. It can easily be had at well supplied veterinary supply stores in the
horse section. It is also sold widely on the internet at a very reasonable price. One must avoid the creams,
and stick to the pure liquid DMSO solvent.
The introduction of procedures using DMSO solvent led to the discovery that this reaction gives very
high yields of the methylcnedioxy derivative of ephedrine and pseudoephedrine if piperonal is used in the
reaction instead of benzaldehyde. This opens up an entirely new way of making MDMA. One could react
piperonal with N-mcthylalanine, and then reduce the product substituted ephedrine with lithium in
anhydrous ammonia to MDMA. One could also use the reduction routes working through
chloroephedrine and palladium. The reduction methods using H I and red P would not work because H I
cleaves ethers on a benzene ring.
Benzaldehyde has been added to the List One of watched chemicals, but check out the " Making
Shitloads of your own Benzaldehyde" section in the "Other Methods of Making Phenylacetone" chapter.
That leaves the N-methylalanine problem. Only N-methylalanine can be successfully be used in this
reaction. Ordinary health food store alanine will react to give I ,2-diphenylethanolamine. N, NChapter
Eighteen
Cooking Your Own Ephedrine
185
dimethylalanine will give no reaction. Check out the Journal of the Phannaceutical Society of Japan Vol.
12, pages 8 1 2 to 8 1 5 ( 1 952) for a complete discussion of these results.
A great stroke of luck for meth cooks was published in 2007. It is a very easy and very high yielding
procedure for making N-methylalanine. It can be found in Tetrahedron Letters, Volume 48, pages 7680-
82. The reaction uses formaldehyde and zinc dust to do the methylation in water solvent containing partly
neutralized phosphoric acid. Formaldehyde can be picked up on the internet or from other sources at low
cost and with no heat attached as of 2009. A little bit goes a long way and the other materials can be
picked off shelves at stores.
The following procedure has been found to be an easy and very productive method tor making Nmethylalanine.
It is given on a 10 gr scale because larger amounts are not done easily with a magnetic
stirrer. The zinc dust is quite dense, but must be kicked up into solution to react.
To 200 ml water in a beaker or other container, add 1 6 ml phosphoric acid. The hardware store dairy
mi IkslOne remover phosphoric would work if account was taken of its weaker strength, and the detergent
extracted. Next add 9.5 gr of NaOH to form the monobasic sodium phosphate. Lye would substitute as
would bicarb or washing soda so long as the amount added was adj usted. Stir constantly. One should be
able to make a roughly equivalent buffer solution by adding 40 grams of hardware store trisodium
phosphate (TSP) to 200 ml of water, and then adding roughly 30 ml of hardware store hydrochloric acid.
I haven't tried this variation, but it should work and would be entirely supplied right off the hardware
store shelf.
Now to this mixture add 1 0 gr alanine (. 1 1 mole) from the health food store. It dissolves quite easily,
and the solution should be around 30 C from the neutralization of the phosphoric acid solution by lye.
Next add 1 0 ml ( . 1 4 mole) 37% tonnaldehyde, follow that with 1 5 gr zinc dust andstir for 45 minutes. I
know that is more than the Tetrahedron Letters article specified, but the amount of formaldehyde has
been backed down from the 1 .5 molar excess stated in that article to around 1 .2. Fonnaldehyde is toxic
and no doubt folks would do it in a kitchen. Less is more ... so increase reaction time ... besides that is the
ingredient that one would need to purchase.
One will note a constant fizzing noise from the reaction vessel as the zinc dust reacts and makes
hydrogen. The zinc gradually changes from grey to blue, and this is zinc phosphate. Zinc dust is easily
had, but one can make one's own by taking a piece of zinc metal such as pennies and grinding on a wheel
or with a file until they are reduced to grit and dust.
Now let the zinc settle, then filter the almost clear water solution leaving the zinc on the bottom of the
flask. It should filter clear water white through a couple of coffee tilters.
Add 50 ml of hot water to the settled blue zinc sludge on the bottom of the flask, and swirl for a bit.
Then let that settle. Filter off the water, and add this to the main charge of filtered water.
Now tor the important part. . . add bicarb powder slowly and with stirring until the p H reaches roughly
pH 7. One will need a pH meter, and make sure it is calibrated. Tap water should read within a few tenths
o f p l l 7, but buffer solutions are easy to get to calibrate a pH meter.
Once the pH has been adj usted to around 7, let the water clear solution sit in the fridge overnight. Great
hcavy masses of long needle shaped N- methyl alanine will form. Let the mass grow to its greatest extent.
It may take more than 1 2 hours to get the crystal growth to kick off. I f one has a seed crystal, it would be
very convenient.
When the crystal mass has stopped growing, filter it off. Then rinse it with some alcohol. .. at least
70'Yo . . . and set the crystals on a plate to dry. The alcohol dries the crystals and keeps them from becoming
bacteria food as they dry. Usc less than 50 mi.
Now the filtered liquid should be boiled down. This is another reason for using less fonnaldehyde.
Boiling the mixture makes the residual formaldehyde become part of the steam given off The mixture
will now be kind of yellow colored. Reduce the liquid volume by half and then add the alcohol rinse from
Secrets or Methamphetamine Manufacture
Eighth Edition
186
the first crop of crystals. Then put this boiled down water liquid in the fridge to collect another crop of
crystals of N-methyl alanine. Total yield is about 1 0 gr after the crystals have dried. This would react
with benzaldehyde in OMSO solvent to give yields of ephedrine and pseudoephedrine which have not
been seen since the mid 90's.
This newer and much better cooking procedure was covered in detail during two conferences sponsored
by the Pharmaceutical Society of Japan in 2006 and 2007. The abstracts were published on line as
"Proceedings of the Symposium on Progress in Organic Reactions and Syntheses". The two papers in
question were presented at the 32"" and 33'd Symposiums by Yokoyama and Tsubaki. The easiest way to
google up these abstracts is by searching 33'd symposium or 32"" symposium. To get the full cooking
details requires some hands on cooking since they are less than willing to give the text of their
proceedings. Go figure on that one!
The preferred procedure is to react one mole of benzaldehyde with two moles of N-methylalanine in
DMSO solvent. Let's take a small scale example using 30 ml of benzaldehyde. It would react with 60
grams ofN-methylalanine to give roughly 25 to 30 grams of a mixture of ephedrine and pseudoephedrine
hydrochloride.
Now place 250 ml of OMSO into a suitable heating vessel such as a round bottom flask with reflux
condenser . . . or a lava lamp if you are ghetto . . . add a magnetic stir bar. . . and 60 gr of N-methyl alanine.
Then add 1 0 ml of the 30 ml of the benzaldehyde. It is best to add it in portions to save on the total
amount of OM SO solvent used. This makes the clean up at the end of the reaction much more practical.
Heat this mixture to about 1 30 C if one is using piperonal, but benzaldehyde will react at a lower
temperature. Look for the fizzing of C02 as your visual clue, and go with the lower temperature. Let it
fizz for an hour or so, then add the next \0 ml portion of the 30 ml total benzaldehyde add. Let it
similarly fizz for an hour before adding the last 1 0 ml portion of benzaldehyde.
After the last addition of benzaldehyde, let the mixture heat at the lowest tizzing temperature, and then
tum up the heat slowly. The max with benzaldehyde should be at about 1 30 C. Piperonal would react
much more easily, but allow the mixture to tizz to complete reation. Take no more than 6 hours on this
stage of the reaction. Just push up the heat to get it going.
Now for the new part of the reaction Uust discovered), "Vinegar", yes the really cheap distilled white
vinegar at the grocery store, greatly increases yield by breaking up a dimer complex the product forms.
At this scale, add 500 to 600 ml of that cheap grocery store vinegar, and swirl to mix it in. Then add from
50 to 1 00 ml of toluene or xylene. This solvent serves as a catcher for the BS we don't want.
You will note that after adding the two volumes of vinegar, the toluene or xylene now form a layer on
top of the DMSO and product layer. This is important as it is the crap catcher. The mixture now must be
heated to reflux boiling temperature for 3 to 6 hours to break up the dimer and give the greater yields one
wants. A lava lamp is unsuitable for this purpose.
Heat the mixture to boiling gently for three to six hours. Then let it cool. This has broken up the dimer.
Add about a shot glass of hardware store hydrochloric acid to the mixture and mix it in. This will assure
that all the ephedrine stays out of the toluene layer.
Now put the reaction into a sep funnel and shake it. Let this settle and the toluene layer on top would
have crap and unreacted benzaldehye in it. Put it aside for further work, the water layer underneath has
the product.
Next base the OMSO and water solution containing the ephedrine and pseudoephedrine. Add a
solution of lye to it with sirring and shaking until the p H is 1 3 plus. This should not take all that much lye
to reach that level. Then add about 1 00 ml of toluene or xylene to extrtact the product. Save it. Extract
again with 50 ml of toluene or xylene.
Chapter Eighteen
Cooking Your Own Ephedrine
187
Wash the combined extracts with some water to rid them of DMSO, then let then sit to shed water and
then transfer to a dry beaker minus the water droplets, and bubble with dry HCL to give about 30 grams
of pure pseudoephedrine and ephedrine mixture as hydrochloride crystals. Keep water out of the dry HCI
bubbling mixture!

hope it is of some use to yall. Thank Uncle fester not me, well you could thank me for cuting`n`pasteing it.............now it time for the customery Tweaker, meth cook (this one is new to me, I'm a newbee from one scourse? sourse one? and trying to build a fake reputation as a meth cook??) WHAT'S THAT ALL ABOUT? CAN ANYONE ENLIGHTEN ME? Xtal
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[*] posted on 10-4-2011 at 22:34


i was just tryng to say to use formalin not formalin and, ammonium chloride because the "recipie" does not call for it.
and very few have had any sucess with reducing the formaldimine of alanine using zinc and formaldehyde because in order to get it to generate hydrides very specific ph requirements have to be meet with the use of phosphate buffers.
and even then sucess is not guaranteed.
i took a cursory glance at the recipie above and i saw no mention of this problem
it looks like some bullshit someone published for the sake of making a buck.
oh it is nevermind.
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[*] posted on 10-4-2011 at 23:18
formalin malachite solution


I can buy 37% formalin with malachite from an aquarium, but there is FUCKING malachite in it and I want to get it out so I can have a pure solution of the formaldehyde.
How do I do this?
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[*] posted on 10-4-2011 at 23:21


Quote: Originally posted by jon  
i was just tryng to say to use formalin not formalin and, ammonium chloride because the "recipie" does not call for it.
and very few have had any sucess with reducing the formaldimine of alanine using zinc and formaldehyde because in order to get it to generate hydrides very specific ph requirements have to be meet with the use of phosphate buffers.
and even then sucess is not guaranteed.
i took a cursory glance at the recipie above and i saw no mention of this problem
it looks like some bullshit someone published for the sake of making a buck.
oh it is nevermind.


:D LMFAO :D Has Fester ever got it right? I allways hear ppl saying they tried the way it was done in the book, but didn't get the same results.
It was the only bit of litriture I could find about it's solubility's
There appears to be a silance surrounding this N protected amino acid, which means it has limited uses?, and would those uses be the usual suspects ( ephedrin, PSE ) If so, I won't waste any more time looking for info on it.
Xtal
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[*] posted on 11-4-2011 at 00:27


well you can try surer means of mono-alkylation for example you could reduce the formaldimine with sodium borohydride.
with the amino acid it is tricky to get the ph spot on to induce hydride formation hydride transfer and so on.
so just use a complex metal hydride and be done with it.

questions: you distill it.
it boils around the boiling point of water.

[Edited on 11-4-2011 by jon]
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[*] posted on 11-4-2011 at 10:36


I don't mind discussion of synthetic routes to N-methylalanine, but this series of posts started badly and went to worse. It should also go in its own thread rather than being tacked on to the Akabori thread.



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