反应详情

To a solution of N-tert-butoxycarbonyl glycine (0.5 g, 2.85 mmol) in dichloromethane (25 ml) at rt was added 3-chloroaniline (0.43 g, 3.42 mmol), HOBt (0.58 g, 4.28 mmol), EDC (1.10 g, 5.7 mmol) and N-methyl morpholine (0.43 g, 4.28 mmol). The reaction was stirred for 5 h and then washed with 1M KHSO4, 10% NaHCO3 solution and brine. The organic phase was separated, dried (Na2SO4), filtered and concentrated under reduced pressure to give [(3-chloro-phenylcarbamoyl)-methyl]-carbamic acid tert-butyl ester (0.7 g, 86%). HPLC-MS 284, 286 [M+1]+.

1. washwashed with 1M KHSO4, 10% NaHCO3 solution and brine
2. customThe organic phase was separated
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure