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Posts 1 - 18 of 18

 Subject: P2P 

 

 

 

 

 

 

obituary
(Hive Addict)
08-16-01 14:50
No 205221

  

  

P2P

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Does anybody know the yeild for this procedure?Method with Benzyl Chloride
Benzyl chloride (PhCH2Cl) and sodium give benzyl sodium. This reacted with ethyl acetate gives phenylacetone. No yield is given in the abstract. Tsuruta, Bull. Inst. Chem. Research, Kyoto Univ., vol. 31, 190-200 (1953) (in English); Chemical Abstracts vol 49, 6183b

 

 

 

 

 

 

Rhodium
(Chief Bee)
08-16-01 16:30
No 205260

  

  

Re: P2P

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Isn't this discussed in the meth forum? And isn't this method described in one of fester's books? If so, where?

 

 

 

 

 

 

WizardX
(Wizard Master)
08-16-01 19:43
No 205312

  

  

Re: P2P

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This is WHY benzylchloride is so highly restricted.

benzylMgCl + acetic anhydride ==>>
P2P  -78oC

benzylNa + CH3COCl(acetyl chloride) ==>>
P2P  95+%

(benzyl)2Zn + 2 CH3COCl(acetyl chloride)==>> 2
P2P + ZnCl2

benzylMgCl + CH3CH=N-CH3 ==H2O==>> Amphetamine

 

 

 

 

 

 

terbium
(Hive Addict)
08-16-01 20:10
No 205318

  

  

Re: P2P

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Really, benzyl chloride is restricted? Even so, I'll bet that benzyl alcohol isn't. A little muriatic acid should serve to convert the alcohol to the chloride.

 

 

 

 

 

 

Rhodium
(Chief Bee)
08-16-01 23:55
No 205368

  

  

Re: P2P

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Wizard: What are the refs for those
P2P production schemes?

 

 

 

 

 

 

WizardX
(Wizard Master)
08-18-01 22:25
No 205777

  

  

Re: P2P

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Will put the refs together.

 

 

 

 

 

 

tecnetium
(Hive Bee)
08-20-01 20:18
No 206192

  

  

Re: P2P

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R- Maybe you could put those synths on your page....Please please please.

PS- Benzyl chloride is easily made from BZOH HCL and a little ZnCl2

 

 

 

 

 

 

Lino
(Hive Bee)
09-06-01 18:17
No 210926

  

  

Re: P2P

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If someBee had a couple a litres of BzCl, but was sick of failed Grignards; he couldn't buy the acetic anhydride. Is there any way the BzCl could be rearranged/reduced… whatever to the aldehyde. SomeBee saw a post by anomolon which claimed benzAl chloride (AKA a,a-dichlorotoluene) could be boiled in alkaline water, to make benzaldehyde (?). That doesn't seem to work w/ BzCl though.

If converting benzAl chloride to benzaldehyde is so simple… I noticed they list a 3,4-dichlorotoluene: I was wondering…


Linoleum: the 13th element!  Now available at all good DIY stores… & Walmart.

 

 

 

 

 

 

obituary
(Hive Addict)
09-06-01 21:29
No 210969

  

  

Re: P2P

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if you use Benzalchloride (dichloromethylbenzene) and boil it with a basic solution the OH will replace both of the halogens to give a dihydroxy-compound (geminal-diol) that will automatically dehydrate (lose water) to give the benzaldehyde

this will work for various sub'd benzaldehydes

 

 

 

 

 

 

Alkylight
(Newbee)
09-06-01 22:54
No 210988

  

  

Re: P2P

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Can't benzylchloride just be treated with hydroxide and then oxidised with say KMnO4 or the likes (but don't go too far-then you get benzoic acid-which can be then converted to
P2P with sodium acetate and acetic anhydride???

 

 

 

 

 

 

terbium
(Hive Addict)
09-06-01 23:13
No 211000

  

  

Re: P2P

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then you get benzoic acid-which can be then converted to P2P with sodium acetate and acetic anhydride???


Really! You have discovered some new chemistry here.

 

 

 

 

 

 

Rhodium
(Chief Bee)
09-07-01 03:24
No 211047

  

  

Re: P2P

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Lino: Reaction of benzyl chloride with hexamethylenetetramine followed by hydrolysis yields benzaldehyde. It is a name reaction, but I have forgotten the name of it.

Alkylight: Benzoic acid won't react that way, but phenylacetic acid will. That's why phenylacetic acid is controlled, but not benzoic acid (which can even be had as the sodium salt in grocery stores as a preservative).

 

 

 

 

 

 

obituary
(Hive Addict)
09-07-01 20:43
No 211268

  

  

Re: P2P

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Rhodium, thanks for the tip on the benzald. synth

do you have any idea what the general pathway is for that rxn?  perhaps a key word to search to find info on that specific rxn? 

 

 

 

 

 

 

terbium
(Hive Addict)
09-07-01 22:59
No 211291

  

  

Re: P2P

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Lino: Reaction of benzyl chloride with hexamethylenetetramine followed by hydrolysis yields benzaldehyde. It is a name reaction, but I have forgotten the name of it.


Sommelet reaction.

 

 

 

 

 

 

obituary
(Hive Addict)
09-08-01 16:57
No 211494

  

  

Re: P2P

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thanks Terbium

 

 

 

 

 

 

tecnetium
(Hive Bee)
09-08-01 19:43
No 211523

  

  

Re: P2P

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Hey Lino

Have you considered making your own Ac2O? It can be made form Br, S and sodium acetate (made form acetic acid and sodium hydroxide)- check out the synth at Rhodiums page.

Also: I recall a grignard reaction that was discussed that made
P2P from BzMgCl and acetonitrile but I can not seem to find any of the old threads- can anyone please give me the reaction details.

 

 

 

 

 

 

jim
(Hive Bee)
09-08-01 21:42
No 211547

  

  

Re: P2P

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An even better way to Ac2O is from acetone via the ketene degradation, see rhodium's website for the link.

 

 

 

 

 

 

Lino
(Hive Bee)
09-13-01 19:23
No 213294

  

  

Re: P2P

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Rh. & terbium: cheers! Vogel's 5th p999-1002. SomeBee sez she's got hexamine and GAA in stock so will give it a go and pass on the results of course. Gimme a month or so as SomeBees goin' to Ibiza!!! Lucky Bee.

tecnetium: didn't fancy all the messin' & coughin' w/Br2. I could buy the fff…sucker but it attracts attention due mostly to it's use in synth of H. Apparently one has to sign End User Cert.
Re. MeCn… bin' there, done that, etc, etc. It doesn't run, not for SomeBee anyhow. Poodle did a 'Right' Up of it (poss on Rh's pg.) but alas Poodles broken English was not clear enough to follow for crucial bits. Sorry Poodle, I'm sure your English is X100 better than Lino's French.

jim: regarding Ac20 from keten. Vogel shows us the device and how to do it on p101. Arthur also mentions in a note "Keten is a poisonous gas having a toxicity comparable with phosgene".
Now: for you younger Bees who don't remember WW1. Phosgene was used by the Germans before they invented mustard gas and…

Errrrrr… does any Bee have experience of 3,4-dichlorotoluene or a,a-dichlorotoluene?


Linoleum: the 13th element!  Now available at all good DIY stores… & Walmart.

 

 

 

 

Posts 1 - 18 of 18  

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