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swip2
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Swip2 dident notice wether diffrent solvents can be used, And whitch ones work better.
Swip2 assumes an avarige non polar solvent would do for the post reaction work up 
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manimal
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Sodium carbonate can be used to base ephedrine or norephedrine, but isn't strong enough to base benzylamine because benzylamine can form a carbonate
salt whereas ppa cannot, no? So wouldn't the addition of a carbonate seperate the ppa as a freebase, but not the benzylamine, which forms a carbonate?
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swip2
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PPA Sulphate or Citrate maybee
| Quote: | Originally posted by IOC
Try alanine/benz, heat directly, when CO2 is done add equal amount of toulene then add equal amount of H2O and acidify to PH 4, seperate water phase
and 3 x methylene chloride to clean.
Boil down H2O pahse to a brown paste then add dry acetone to leave clean white powder.
Havnt had time to qualify MP, next time though
IOC......out |
So how about a PPA Sulphate or a citrate salt.
Swip2 just isent sure weather a sulphate salt would reduce to the desired amine
[Edited on 18-2-2008 by swip2]
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Nicodem
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From here on no more schizophrenic third person writing or use of acronyms of the SWIM-type will be allowed. Any other methods of posing or
pretending of being involved in some criminal activities, or similar childish attempts at being kewl, are also not desired.
Any post not respecting the above will be deleted.
This warning is valid in general and not just this thread.
This used to be a very nice and informative thread about an interesting reaction. Do not deteriorate it! If you have nothing useful to add, then
rather think twice before posting.
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Ephoton
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Mood: trying to figure out why I need a dark room retreat when I live in a forest of wattle.
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sorry tar.gz was ment to mean tar ball  I was in a hurry and should have thought
more about my post.
e3500 console login: root
bash-2.05#
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stoichiometric_steve
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i was about to complain, too. maybe some cleanup should be done here. from page 2 it's mainly bullshit being posted.
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LSD25
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| Quote: | Originally posted by Nicodem
From here on no more schizophrenic third person writing or use of acronyms of the SWIM-type will be allowed. Any other methods of posing or
pretending of being involved in some criminal activities, or similar childish attempts at being kewl, are also not desired.
Any post not respecting the above will be deleted.
This warning is valid in general and not just this thread.
This used to be a very nice and informative thread about an interesting reaction. Do not deteriorate it! If you have nothing useful to add, then
rather think twice before posting. |
Done,
All non-informative and cookery related material that I have access to is now deleted and will not return.
This should please Sauron & Polverone no fucking end.
Out
Whhhoooppps, that sure didn't work
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Nicodem
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I don't know what you are up to, but your posts were one of the few here that did not fit the criteria for removal. Besides, the warning was set for
19/2/2008 and forward and not for already posted material. Take notion that his is not a thread where you can demonstrate your political opinions by
performing irrational acts!
Edit: Now that I think of it, you are actually trying to be kewl if the definition of kewlness is stretched a bit. Maybe your above post actually
breaks the anti-kewls rule after all. I'll have to think about it and perhaps remove it.
[Edited on 25/2/2008 by Nicodem]
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azo
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akabori
I was looking at the akabori reaction and come up with the idea of reacting phenylalinine with formilin the reaction seems to follow the same
mechanism as the benz method only that the end product would be 1 phenyl 2 amino propane 3 ol . The only thing that i thought would be getting the
temperature high enough to decarboxylate the phenylalinine due to the boiling point of water
and the reactivity of the formaldehyde which is a lot more reactive than benzaldehyde
if it would work i thought it would give a better yield due to the solubility of phenylalinine and formilin and easier for the workup with less tar.
has anyone seen this reaction before and do you think it is possable
regard azo
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Maja
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Retried Akabori reaction with Benzaldehyde and Alanine... This time I used overhead stirrer and kept temperature 150-165* for about 2hours. Some
benzylamine and other products distilled over 2hours, but not a lot of. OK ... This is phase were I faced some problem.. Tried to extract with
toluene... And guess what ? No layers ... Just brown solution with no layers. Emulsion ? I don't think so... Maybe someone knows how to solve this
problem ?
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Hilski
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| Quote: | Originally posted by Maja
Retried Akabori reaction with Benzaldehyde and Alanine... This time I used overhead stirrer and kept temperature 150-165* for about 2hours. Some
benzylamine and other products distilled over 2hours, but not a lot of. OK ... This is phase were I faced some problem.. Tried to extract with
toluene... And guess what ? No layers ... Just brown solution with no layers. Emulsion ? I don't think so... Maybe someone knows how to solve this
problem ? |
There really aren't any layers. The toluene is mostly to thin things out a bit so it will be easier to filter out the unreacted alanine and maybe
some tar etc. The last time I tried this (quite a while back) I just filtered the thinned solution a few times to clean it up as much as possible
and then added water and HCL to extract the reaction product. That's really the only time I saw any kind of layers form. I never really had much of
a tar layer at the bottom.
Once the water has been evaporated, the amine salt is left behind as a dirty paste (Just like in the photos) and is kind of a bitch to clean up, but
it can be done.
As an aside, I seem to remember having VERY strong ammonia-like vapors coming from the reaction solution. I'm not sure if this was from a lot of
benzylamine (or other side products) forming, or if it was just from the amine that that was the desired product of the reaction.
**I almost forgot...After the aqueous layer has been separated, be sure to wash it several times as well as you can with a non-polar solvent. DCM
definitely works best for this if you have it. Otherwise it'll take a ton of ethyl acetate to clean up the paste at the end.
Pretty much everything Cycloknight put in his write up works the way he says it does if you follow his procedures.
[Edited on 29-4-2008 by Hilski]
\"They that can give up essential liberty
to obtain a little temporary safety
deserve neither liberty nor safety. \"
- Benjamin Franklin
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azo
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? what isomer is produced by the akabori is it norephedrine
or norpseudoephedrine.
I haven't heard it mentioned
thanks azo.
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Maja
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Oh, I see... So why does he state that you need to extract with toluene ? :] I will try what you said. I have DCM. I don't actually remember from the
past if there was layers or no ..
I think it's norpseudoephedrine if IIRC :]
[Edited on 29-4-2008 by Maja]
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Hilski
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| Quote: | Oh, I see... So why does he state that you need to extract with toluene ? :] I will try what you said. I have DCM. I don't actually remember from the
past if there was layers or no ..
I think it's norpseudoephedrine if IIRC :] |
I'm not really sure why he used the term 'extract' when referring to the procedure right after the reaction completes. I believe it's just semantics,
and I THINK what he was intending to convey was that one just needs to add toluene to the final reaction mixture. Then filter out the unreacted
alanine and wash the alanine with some clean toluene to make sure no product is left behind. Then pool all the toluene together to do the the
extraction on the toluene with aqueous HCL.
If I'm not mistaken, the reaction product is a mixture of d- and l- norephedrine, a.k.a phenylpropanolamine. There might also be some norephedrine in
there too, but I don't think so.
\"They that can give up essential liberty
to obtain a little temporary safety
deserve neither liberty nor safety. \"
- Benjamin Franklin
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jon
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benzylamine is only formed about 1-3% it is soluble in h2o completely not an issue. diphenylethanolamine is insoluble in alcohol as a base per a
scientist at sigma aldrich .6g/100ml with heavy sonification. this is the major impurity.
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Hilski
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So Maja, any luck? I'm just curious, because I don't remember reading any posts by anyone other than Cycloknight who actually tried the experiment
and got it to work . IIRC I ended up with %15-%20 yields (based on benzaldehyde) when I did it last.
\"They that can give up essential liberty
to obtain a little temporary safety
deserve neither liberty nor safety. \"
- Benjamin Franklin
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HeilHamas
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| Quote: | Originally posted by jon
I've given the serine route a thought but after some research I concluded it may or may not be possble because of the steric factors involved with
alanine the carbon bearing the alpha hydrogen is substituted in alanine in the case of glycine it is not.
[Edited on 23-12-2007 by jon] |
It's been demonstrated to work for alanine and nitrobenzaldehyde in an uncatalyzed reaction. Nitrobenzaldehyde is more reactive in such reactions, but
if steric hinderance doesnt hinder alanine and nitrobenzaldehyde, why would it hinder alanine and benzaldehyde? It should be tried in a standard
base-catalyzed reaction.
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chochu3
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PPA*HCl
very sol. H2O
sol. Alcohol
insol. ether, benzene, chloroform
PPA freebase
sol. ether
Alanine
sol. H2O
slightly sol. Alcohol, pyridine
insol. Acetone, ether
Best way to workup this reaction would be to do the extraction with ether so it will solvate the PPA and leave the alanine behind. Referenced from
Handbook of Chemistry and Physics 85th edition except the solubilty of the phenylpropanolamine freebase which was read from a patent online here
\"Abiding in the midst of ignorance, thinking themselves wise and learned, fools go aimlessly hither and thither, like blind led by the blind.\" -
Katha Upanishad
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hector2000
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there is no way for convert ppa to pesudoehedrine?
i think if we use methyle alanine then we will have pesudoephedrine
Chemistry=Chem+ is+ Try
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hector2000
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why final product has tart and bitter taste?
Chemistry=Chem+ is+ Try
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sk13m11
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l-alanine to ppa
can i use beta-alanine instead of l-alanine
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Siddy
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@ sk13m11 - You can use l-alanine, d-alanine or dl-alanine. NOT BETA (B)!
@ hector2000 - The original Akabori (and MOMOTANI) paper trials n-methyl alanine (thats the whole point of the paper, semi synthetic ephedrine). They
got 16% with there method which uses pyridine. The methods you read on this site increase the yield and dont use pyridine. Although since n-methyl
alanine is not commercially available no one as tried it since Akabori...
You can methylate an amine (single methylation) with formaldehyde and a reducing agent.
Products via this method are racemic (4 different isomers).
[Edited on 27-3-2009 by Siddy]
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sk13m11
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thanks for the info
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unome2
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Sorry, under a new pseudonym (while I try and find my original activation email - I suspect it is in an account which has been heavily spammed).
Found this the other day, it is in Japanese too, but it at least shows a putative reaction scheme (via an acid labile, 5 membered ring).
Interestingly, it claims that the 3,4-MD benzaldehyde (piperonal) gives up to 87% yield while plain old benzaldehyde gives only <50% (which is
likely, given that it forms two sides of the 5 membered ring).
The references from this paper really ought to be rather special reading if anyone can find them too
Attachment: akabori.rewrite.2007.pdf (94kB)
This file has been downloaded 1776 times
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Siddy
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good find no1uwant2no,
You can get a ruff translation from google, and make sense of it.
But it doesnt detail the method, or say how the yield was increased.
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