反应详情

Triethylamine (0.012 mL, 0.084 mmol) was added to a solution (3R,6S)-3-amino-6-(2,3-difluorophenyl)-1-(2-methoxyethyl)azepan-2-one (25 mg, 0.084 mmol) and p-nitrophenyl chloroformate (25 mg, 0.126 mmol) in tetrahydrofuran (1 mL) at 0° C. After 0.5 h, triethylamine (0.036 mL, 0.252 mmol) and 4-phenyl-1-piperidin-4-yl-imidazolidin-2-one (31 mg, 0.126 mmol) were added and the mixture was allowed to warm to ambient temperature. After 1 h, the mixture was quenched with water, extracted with dichloromethane, and washed with 1 N NaOH solution. The combined organic layer was dried over sodium sulfate, filtered, and concentrated. Purification by silica gel chromatography (0.5% methanol/dichloromethane→6% methanol/dichloromethane) gave the title compound (11 mg). MS 570.3 (M+1).

1. waitAfter 1 h
2. customthe mixture was quenched with water
3. extractionextracted with dichloromethane
4. washwashed with 1 N NaOH solution
5. dry with materialThe combined organic layer was dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification by silica gel chromatography (0.5% methanol/dichloromethane→6% methanol/dichloromethane)