Реакция #1994242

Уравнение реакции

L-glutamic acid

acetic anhydride

KOH

triethylamine

→

N,5-diacetylpyrrolidin-2-one

Условия реакции

Обработка

1. 1
   ДругоеThe crude reaction product
2. 2
   Концентрированиеis concentrated under reduced pressure (rotary evaporator and vane pump)
3. 3
   Промывкаthe organic layer is then washed five times with 100 mL of deionized water
4. 4
   workup.ADDITIONtreated over animal carbon
5. 5
   ДругоеThe product obtained
6. 6
   Другоеafter evaporation of the solvent
7. 7
   Другоеis purified by crystallization from petroleum ether/CH2Cl2
8. 8
   ПромывкаThe crystals are rinsed with petroleum ether

Методика

A 500-mL round bottom flask under argon atmosphere is charged with L-glutamic acid 4 (21 g, 0.143 mol), a catalytic amount of N,N-dimethylaminopyridine (150 mg, 1×10−3 mol), acetic anhydride (75 mL) and triethylamine previously distilled over KOH (75 mL). The reaction mixture is maintained at 60° C. for 16 hours. The progression of the reaction is followed by TLC (eluent: ethyl acetate/petroleum ether at a ratio of 8/2). The crude reaction product is concentrated under reduced pressure (rotary evaporator and vane pump) and then taken up in 200 mL of dichloromethane; the organic layer is then washed five times with 100 mL of deionized water and then treated over animal carbon. The product obtained after evaporation of the solvent is purified by crystallization from petroleum ether/CH2Cl2. The crystals are rinsed with petroleum ether.

Источник