反应详情

温度

60 °C

Sodium hydride (0.36 g, 60% in oil) was added to 20 ml of dimethyl sulfoxide (DMSO) and stirred at 60° C. for one hour. Subsequently, 2.0 g of 3,4-dichlorophenyl-phenylamine was added to the mixture and stirred at 60° C. for one hour. A DMSO solution containing 1.5 g of 3(R)-methanesulfonyloxypyrrolidine-1-carboxylic acid tert-butyl ester was gradually added to the mixture and stirred at 60° C. for 15 hours. Ethyl acetate was added to the reaction solution, and the reaction solution was then washed with water and dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1). The eluent solvent was distilled off under reduced pressure to thereby obtain 0.13 g of light brown amorphous solid 3(S)-[(3,4-dichlorophenyl)phenylamino]pyrrolidine 1-carboxylic acid tert-butyl ester.

1. stirringstirred at 60° C. for one hour
2. additionwas gradually added to the mixture
3. stirringstirred at 60° C. for 15 hours
4. washthe reaction solution was then washed with water
5. dry with materialdried over magnesium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1)
8. distillationThe eluent solvent was distilled off under reduced pressure