反应详情

To 9-tert-butoxycarbonylamino-3-cyclohexylmethoxy-6,7,8,9-tetrahydro-5H-benzocycloheptene-2-carboxylic acid (1.5 g, 3.60 mmol) in CH2Cl2/DMF (4:1, 25 mL) was added HOBT (0.53 g, 4.0 mmol) and EDC (0.76 g, 4.0 mmol) and the mixture allowed to stir for 30 min. To this was added NH4OH (27% aqueous, 0.30 mL, 4.0 mmol) and stirring was continued for 3 h. The mixture was diluted with 1 M HCl and extracted with EtOAc. The combined extracts were washed with water, sat'd NaHCO3, dried over magnesium sulfate,and concentrated to a solid. The solid was recrystallized from Et2O to yield a white solid (5.0 g, 68%). MS [M−H]− 415, m.p. 193-194° C.

1. stirringstirring
2. waitwas continued for 3 h
3. extractionextracted with EtOAc
4. washThe combined extracts were washed with water
5. dry with materialdried over magnesium sulfate,and
6. concentrationconcentrated to a solid
7. customThe solid was recrystallized from Et2O