反応 #1994242

反応方程式

L-glutamic acid

acetic anhydride

KOH

triethylamine

→

N,5-diacetylpyrrolidin-2-one

反応条件

後処理

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

実験手順

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.

出典