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	Posts 1 - 13 of 13	Subject: Another P2P Synthesis



Wizard X (Moderator) 02-11-00 20:29 No 118170	Another P2P Synthesis	Bookmark Reply
	C6H5CH2MgBr + CH3CO2Na ====[ether/25degC/24Hrs]======> C6H5CH2-C(=O)-CH3 + NaOMgBr P2P is only 25% C6H5CH2Li + CH3CO2Li ====[ether/25degC/6Hrs]======> C6H5CH2-C(=O)-CH3 + Li2O P2P is only 62-63% C6H5CH2CO2Li + CH3Li ====[ether/25degC/2-3Hrs]======> C6H5CH2-C(=O)-CH3 + Li2O P2P is only 69%



Uncle Fester (Member) 02-13-00 14:28 No 118171	Re: Another P2P Synthesis	Bookmark Reply
	If I were cooking now, and the heat didn't know who I was, so I could get some breathing room, the method I would check out is in J. Org. Chem. Vol 28 pages 879-81. One heats a mixture of phenylacetic, acetic acid and iron powder, and distills out the phenylacetone.



born_slippy (Member) 02-13-00 14:59 No 118172	Re: Another P2P Synthesis	Bookmark Reply
	can you give a write up for C6H5CH2MgBr + CH3CO2Na ====[ether/25degC/24Hrs]======> C6H5CH2-C(=O)-CH3 + NaOMgBr P2P is only 25%



Xaja (Member) 02-13-00 17:26 No 118173	Re: Another P2P Synthesis	Bookmark Reply
	Uncle Fester: If you have time could you please post the details to that? It would be cool to find a way around PAA, this is the real *bitch!* But might as well avoid AA in the meanwhile. Wizard X, grignards looks good, wouldn't mind seeing that writeup either.



Uncle Fester (Member) 02-13-00 17:35 No 118174	Re: Another P2P Synthesis	Bookmark Reply
	If I wanted to go into industrial scale production, I'd get a drum of ethylbenzene and do the chromate oxidation to PAA(yield 90%) given in Advanced Techniques. Once one has PAA, the rest is a cakewalk. For the J. Org Chem article, I suggest a walk to the library. It's a very healthy alternative to sitting in front of a screen.



Xaja (Member) 02-13-00 18:18 No 118175	Re: Another P2P Synthesis	Bookmark Reply
	OK, OK. I suppose I should do something for myself sometimes. Thanx for the PAA info. I guess that's a simple oxidation with Jones reagent.



Wizard X (Moderator) 02-13-00 19:30 No 118176	Re: Another P2P Synthesis	Bookmark Reply
	Uncle Fester: Here is a better method. 1 mole PAA + 3 moles GAA == activated Al2O3/ heat to Bp of P2P ==>> C6H5CH2-C(=O)-CH3 + CH3-C(=O)-CH3 The neutral activated Al2O3 is add to the mixture of 1 mole PAA + 3 moles GAA so a semi-fluid slurry is formed. Then heat to Bp of P2P and distil the P2P + acetone mixture.



Wizard X (Moderator) 02-13-00 19:41 No 118177	Re: Another P2P Synthesis	Bookmark Reply
	Uncle Fester: The method you stated, "ethylbenzene and do the chromate oxidation to PAA(yield 90%) given in Advanced Techniques", did this come from this Ref J.Org. Chem. Vol 34, Pg 1493 (1969).



Uncle Fester (Member) 02-13-00 21:27 No 118178	Re: Another P2P Synthesis	Bookmark Reply
	J. Org Chem vol 62 pages 27-28. Sodium dichromate in water solution plus ethylbenzene. Mixture heated in a sealed steel vessel with agitation .



Xaja (Member) 02-13-00 21:54 No 118179	Re: Another P2P Synthesis	Bookmark Reply
	No H2SO4?



Wizard X (Moderator) 02-13-00 22:42 No 118180	Re: Another P2P Synthesis	Bookmark Reply
	Uncle Fester: Thanks ! The procedures in both Ref's outline the same method.



KrZ (Member) 02-13-00 23:51 No 118181	Re: Another P2P Synthesis	Bookmark Reply
	PLEASE mention my dehydrohalogenation, it's 86% to allylbenzene and you can get 90% conversion to P2P after that! That's 77% overall, and it's very easy and very scalable!



Wizard X (Moderator) 02-14-00 04:57 No 118182	Re: Another P2P Synthesis	Bookmark Reply
	KrZ: Can you email me that one, I must have missed it. Thanks.

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