反应详情

N-(2-mercapto-3-methoxybenzoyl)-N-cyclopentylglycine (14.5 g, 0.0469 m) and triethylamine (4.7 g, 0.0469 m) in methylene chloride (500 ml) were cooled to 0° C., and ethyl chloroformate (5.1 g, 0.0469 m) was added over one minute. The mixture was stirred 2 hours at 0°-10° C., washed (water, then brine), dried (Na2SO4) and concentrated. HPLC purification using hexane/ethyl acetate (1/1) as eluent gave the desired product. Recrystallization from ethyl acetate provided 5.4 g analytically pure material (yield: 35%).

1. washwashed (water
2. dry with materialbrine), dried (Na2SO4)
3. concentrationconcentrated
4. customHPLC purification