Reaktion #1994242

Reaktionsgleichung

L-glutamic acid

acetic anhydride

KOH

triethylamine

→

N,5-diacetylpyrrolidin-2-one

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle