Author Topic: New Old Amph synth?  (Read 7408 times)

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Chemikaze

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New Old Amph synth?
« on: December 06, 2001, 01:11:00 PM »
Whaddya think about this???? ::)
Toluene+MnO2+H2SO4 --> Benzaldehyde + nitroethane -->Nitropropane + LAH --> Amphetamine ????
Well???

Stay 8)

Everybody in the house with a half an ounce
Not weed I meant coke dumb ass sit down!

foxy2

  • Guest
Re: New Old Amph synth?
« Reply #1 on: December 06, 2001, 02:16:00 PM »
Well I am in a better mood now so I'll make this post a little more friendly  :P
The discussion has gotten much better than the initial post would indicate.  However I still don't think there is anything "novel" here, the chemistry forum would have been a better choice.


These procedures are the most basic sythesis of amphetamine there is.  Although I am not familar with the benzaldehyde synthesis it looks like it will work but I doubt the yeild is all that good.


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Rhodium

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Re: New Old Amph synth?
« Reply #2 on: December 06, 2001, 03:27:00 PM »
Yes, the reaction would work precisely as you describe. Do you have any detailed information about the preparation of benzaldehyde from toluene using MnO2?

Chemikaze

  • Guest
Re: New Old Amph synth?
« Reply #3 on: December 06, 2001, 04:09:00 PM »
2 foxy: As you could see the topic name was NEW OLD... By this i meant that the new is the substance (toluene) which is actually new to be an amph precursor.Am i right??

2 Rhodium: Yes,but it is not actually detailed,the procedure itself is easy as hell,the most unpretty part in it is the MnO2 which have to be in activated form,but there is a procedure (not complicated) to turn it to activated form,it was given today by Antoncho,i`ll have to translate it...well it`s not detailed,noone actually tried it seriously...

Everybody in the house with a half an ounce
Not weed I meant coke dumb ass sit down!

Chemikaze

  • Guest
Benzaldehyde via MnO2 oxidation of toluene
« Reply #4 on: December 06, 2001, 04:34:00 PM »
Sorry for my english.


Preparation of benzaldehyde via oxidation of toluene by MnO2 in acidic environment.

Reaction speeds up if you add some HNO3 as a catalyst.

Parts by weight.

To the mixture of 180 parts toluene,1020 parts 65% H2SO4 and 1,2 parts of HNO3,during vigorous stirring is added in portions so that it dissolves, 70 parts of MnO2 (65% of which is activated MnO2,if the percent of activated MnO2 is higher,then you should take less amount), keeping the temperature of reaction mixture near 18-19 C.

When all MnO2 is added,the mixture is stirred for additional 30 minutes, then organic layer is separated from lower aqueous layer (which is MnSO4+H2SO4) and benzaldehyde is separated with steam distilling,and then purified with bisulfite.

The yield is 16 parts, which is 56% of theoretically possible according to activated MnO2.The unreacted toluene can be returned back. The disadvantage is a large amount of H2SO4...

This was uploaded by anonymous guy...
______________________________________

...Preparation of activated MnO2...

Ask Antoncho actually,cause this has to be tweaked...

But it`s easy...

I guess this is really amph from shit.

Good luck.

P.S. There are couple of patents concerning this question in Russian,i can translate them later if you want.
There are couple in German also DRP 107722 (1899)
DRP 101221 (1898). 8)

Everybody in the house with a half an ounce
Not weed I meant coke dumb ass sit down!

Chemikaze

  • Guest
Re: New Old Amph synth?
« Reply #5 on: December 06, 2001, 04:54:00 PM »
Ooops,sorry my fuckup,there are no Russian patents,it was a book 8)

P.S. May be you know this one already...
Us patent "PROCESS FOR PREPARING AROMATIC ALDEHYDES AND KETONES",

Patent US4146582

. The reference was given by Vitsh. It`s not actually using MnO2 and is somewhat more "complicated" but still good one.

bottleneck

  • Guest
Re: New Old Amph synth?
« Reply #6 on: December 06, 2001, 05:51:00 PM »
You can oxidize toluene to benzaldehyde by other means, for example electrolytically.

Rhodium

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Re: New Old Amph synth?
« Reply #7 on: December 06, 2001, 06:11:00 PM »
Chemikaze: Do you have the reference for that procedure, or is that unknown?

Chemikaze

  • Guest
Re: New Old Amph synth?
« Reply #8 on: December 06, 2001, 06:22:00 PM »
This was just uploaded to our forum by Garin.

Preparation of Activated MnO2.(According to Morton)

Mix equivalent quantity of MnO2 and KMnO4 in aqueous solutions, the wash and dry the residue.

Preparation of Activated MnO2 (according to Attenboro).This one is more active.

Solutions of MnSO4 and NaOH are added simultaneously to the stirring solution of KMnO4, the percipitations is separated and washed until the liquid with wich it washed becomes colorless.Solid product is dried under 100-120 C and then finely powered.In typical oxidation 1 gr of secondary alcohol (sorry i`m not sure if i translated this right) in 50ml of petroleum ether is shaked with 1 gr of MnO2 during 1 hour.Distilling yields 0,8 gr of ketone.
This method of oxidation is common to allyl alcohols,primary and secondary as well,and also for alcohols of this type RC=CCH(OH)R`. There is actually triple bond,but i don`t know how to depict it here...

This was taken from the book.

That`s it !

P.S. If someone is interested in oxidation of vitamine A1,just say:)))

Everybody in the house with a half an ounce
Not weed I meant coke dumb ass sit down!

Chemikaze

  • Guest
Re: New Old Amph synth?
« Reply #9 on: December 06, 2001, 06:24:00 PM »
Yes i could ask for that,but it`s not the same what i posted here,i can get a reference for another similiar procedure,it`s almost the same in Russian.

Everybody in the house with a half an ounce
Not weed I meant coke dumb ass sit down!

foxy2

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Re: New Old Amph synth?
« Reply #10 on: December 06, 2001, 08:18:00 PM »
"2 foxy: As you could see the topic name was NEW OLD... By this i meant that the new is the substance (toluene) which is actually new to be an amph precursor.Am i right??"

Ummm, No
There is nothing new about starting with toluene to produce amphetamine, methamphetamine or benzaldehyde.  The procedure for making activated MnO2 is a nice addition.  If only someone had a reference for the oxidation.

See these threads

Post 208702

(Antoncho: "The easiest synth of benzaldehyde from toluene", Chemistry Discourse)

Post 224776

(fructose: "P2P - 100% OTC !?!", Chemistry Discourse)



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Chemikaze

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Re: New Old Amph synth?
« Reply #11 on: December 06, 2001, 10:32:00 PM »
Yes,yes that`s why i arose this topic,cause in the days of those posts there were no certain procedure for benzaldehyde from toluene - no details at all.And today we`ve got all we needed ;D  ;D  ;D .

Now just have to wait for results of Zn-HCL for amphetamines? May be anyone have info on that?

Everybody in the house with a half an ounce
Not weed I meant coke dumb ass sit down!

PolytheneSam

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Re: New Old Amph synth?
« Reply #12 on: December 07, 2001, 12:48:00 AM »

Post 208702

(Antoncho: "The easiest synth of benzaldehyde from toluene", Chemistry Discourse)

The patents I listed are the ones you want to look at for MnO2 + H2SO4.

Post 208782

(PolytheneSam: "Re: The easiest synth of benzaldehyde from toluene", Chemistry Discourse)


http://www.geocities.com/dritte123/PSPF.html


Bwiti

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"benzaldehyde is separated with steam ...
« Reply #13 on: June 08, 2002, 04:52:00 PM »
"benzaldehyde is separated with steam distilling,and then purified with bisulfite."

  It can be used to purify benzaldehydes as well? Sweet! Would one go about this in the same manner as with ketones? 8)


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PrimoPyro

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Yes. :-)
« Reply #14 on: June 08, 2002, 04:53:00 PM »
Yes.  :)

Rhodium

  • Guest
Bisulfite can be used to purify most aldehydes ...
« Reply #15 on: June 08, 2002, 08:29:00 PM »
Bisulfite can be used to purify most aldehydes and ketones.