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All posts Subject: PAA -> P2P 76% yield Please login to post

Dope_Amine
(Hive Bee)
11-07-04 22:22
No 540244
User Picture PAA -> P2P 76% yield
(Rated as: good idea!)

Due to poverty, a bee had to lower her morals and turn into a wasp... She did use less AA and got a higher yield due to some variation of procedure.
86 g Phenylacetic Acid
800 mL Acetic Anhydride (fresh)
43 g sodium acetate
Oven dried molecular sieves

In a three neck 1 L flask fitted with a nitrogen purge line and a thermometer, all above were quickly thrown in while under a stream of N₂. The flask was then fitted with a water condenser with a drierite drying tube. The N₂ purge was slowed to minimal positive pressure and the oil bath heated for 46 hrs to ~170°C, such that rxn temp was ~145°C. Reflux and gas evolution was slight. Color slowly went from clear to yellow. Afterward, solution was rotovaped down to about 300-400 mL dissolved in ~200 mL DCM and stirred vigorously with and excess of 4M NaOH, until no more hydrolysis (noted by vigorous bubbling) occurred. Organic layer separated, aqueous extracted 3 x with DCM, pooled extracts dried w/ mag sulfate, filtered (which also got rid of some insoluble junk) and rotovaped off DCM. Yield 64.4 g (76%), very pure by ¹H-NMR and TLC.

Reasoning for higher yield: fresh (not wet) AA, continuous positive pressure of N₂, drying tube, and mol seives = very dry rxn

*Please don't PM Dopey any questions about this procedure.

something for your mind.......

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	All posts		Subject: PAA -> P2P 76% yield		Please login to post


		Dope_Amine (Hive Bee) 11-07-04 22:22 No 540244				PAA -> P2P 76% yield (Rated as: good idea!)
						Due to poverty, a bee had to lower her morals and turn into a wasp... She did use less AA and got a higher yield due to some variation of procedure. 86 g Phenylacetic Acid 800 mL Acetic Anhydride (fresh) 43 g sodium acetate Oven dried molecular sieves In a three neck 1 L flask fitted with a nitrogen purge line and a thermometer, all above were quickly thrown in while under a stream of N₂. The flask was then fitted with a water condenser with a drierite drying tube. The N₂ purge was slowed to minimal positive pressure and the oil bath heated for 46 hrs to ~170°C, such that rxn temp was ~145°C. Reflux and gas evolution was slight. Color slowly went from clear to yellow. Afterward, solution was rotovaped down to about 300-400 mL dissolved in ~200 mL DCM and stirred vigorously with and excess of 4M NaOH, until no more hydrolysis (noted by vigorous bubbling) occurred. Organic layer separated, aqueous extracted 3 x with DCM, pooled extracts dried w/ mag sulfate, filtered (which also got rid of some insoluble junk) and rotovaped off DCM. Yield 64.4 g (76%), very pure by ¹H-NMR and TLC. Reasoning for higher yield: fresh (not wet) AA, continuous positive pressure of N₂, drying tube, and mol seives = very dry rxn *Please don't PM Dopey any questions about this procedure. something for your mind.......

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