反应详情

To a cooled solution of chlorosulfonyl isocyanate (315 mg, 2.22 mmol) in CH2Cl2 (8 mL) is added dropwise a solution of t-butanol (165 mg, 2.22 mmol) in CH2Cl2 (1 mL). The solution is stirred at RT for 45 min and re-cooled, then a solution of [2-benzyloxy-4-(7-oxo-azepan-2-ylmethyl)-phenylamino]-acetic acid methyl ester (600 mg, 1.48 mmol) and triethylamine (252 mg, 2.52 mmol) in CH2Cl2 (2 mL) is added dropwise. The mixture is stirred at RT for 3 h then washed with water. The organic phase is dried over Na2SO4 and the solvent is removed under reduced pressure. The residual oil is purified by flash chromatography using EtOAc/CH2Cl2 (1:1) as eluent to give the title compound.

1. temperaturere-cooled
2. stirringThe mixture is stirred at RT for 3 h
3. washthen washed with water
4. dry with materialThe organic phase is dried over Na2SO4
5. customthe solvent is removed under reduced pressure
6. customThe residual oil is purified by flash chromatography