反应详情

A solution of pyrrolidine-1,2(S)-dicarboxylic acid 1-t-butyl ester (50 g, 233 mmol), EDC (45 g, 233 mmol) and HOBT (12 g, 77.5 mmol) in 1500 ml of dichloromethane was cooled to 0° C. and aniline (21 ml, 233 mmol) was added dropwise over a period of 15 minutes. The mixture was stirred over night, evaporated and partitioned between ethyl acetate and 1N-HCl. The organic layer was washed with saturated sodium bicarbonate solution and brine, dried over anhydrous sodium sulfate and evaporated. The crude solid was crystallized from diethyl ether. Yield: 104 g (quantitative).

1. customevaporated
2. custompartitioned between ethyl acetate and 1N-HCl
3. washThe organic layer was washed with saturated sodium bicarbonate solution and brine
4. dry with materialdried over anhydrous sodium sulfate
5. customevaporated
6. customThe crude solid was crystallized from diethyl ether