반응 #342792

반응 방정식

acetyl chloride

methanol

L-glutamic acid

→

γ-methyl L-glutamate

용매

pyridine

반응 조건

후처리

1. 1
   기타to stand at room temperature
2. 2
   workup.STIRRINGwith intermittent shaking for 24 hours
3. 3
   기타to form
4. 4
   기타the precipitate was collected on sintered glass
5. 5
   세척washed with two 600 ml portions of ethanol
6. 6
   기타The precipitate was dried in vacuo at room temperature for 3 hours
7. 7
   workup.WAITin a vacuum desiccator over Drierite® for 5 hours
8. 8
   기타was further triturated with ether
9. 9
   기타dried again

실험 절차

A cold solution of 300 ml of acetyl chloride was slowly added to a flask containing 3 liters of methanol. To this mixture was added 442 g of L-glutamic acid. The flask was stoppered and shaken for several minutes to effect solution. The flask was then allowed to stand at room temperature with intermittent shaking for 24 hours. 300 ml of pyridine was added causing a precipitate to form. Upon standing for an additional 48 hours, the precipitate was collected on sintered glass and washed with two 600 ml portions of ethanol and a 250 ml portion of ether. The precipitate was dried in vacuo at room temperature for 3 hours and then in a vacuum desiccator over Drierite® for 5 hours. Pyridine vapors were still perceptible from the precipitate which was further triturated with ether and dried again yielding 201.5 g of the desired γ-methyl L-glutamate as white, shiny plates, m.p. 168°-169° C.

출처