反应详情

To a solution of 4-benzyloxycarbonylamino-cyclohexanecarboxylic acid (8.0 g, 28.78 mmol) in DCM (35 mL) and DMF (35 mL) is added t-butanol (10 mL, 105.4 mmol) and DMAP (1.4 g, 11.50 mmol). DIPC (10 mL) is added portionwise over 1 h. The resulting mixtures stirs 18 h. The mixture is mounted onto SiO2 and purified by flash chromatography (gradient elution: 0-60% EtOAc/Hep) which affords 5.2 g of 4-benzyloxycarbonylamino-cyclohexanecarboxylic acid tert-butyl ester. 1H NMR (400 MHz, DMSO-D6) δ ppm 1.14 (m, 2H) 1.30 (m, 2H) 1.38 (m, 9H) 1.82 (m, 4H) 2.07 (m, 1H) 3.20 (m, 1H) 3.47 (m, 3H) 4.99 (m, 2H) 7.27 (m, 5H).

1. customThe resulting mixtures stirs 18 h
2. custompurified by flash chromatography (gradient elution: 0-60% EtOAc/Hep) which