반응 #1994242

반응 방정식

L-glutamic acid

acetic anhydride

KOH

triethylamine

→

N,5-diacetylpyrrolidin-2-one

반응 조건

후처리

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

실험 절차

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.

출처