HRID271934
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Trifluoroacetic acid (2.5 mL) was added to a solution of tert-butyl (3R,6S)-6-(2,3-difluorophenyl)-1-(2-methoxyethyl)-2-oxoazepan-3-ylcarbamate (99 mg, 0.248 mmol) in dichloromethane (5 mL). After 1 h, the solution was concentrated and azeotroped with toluene (2×). Saturated aqueous sodium bicarbonate solution was added and the mixture was extracted with dichloromethane (3×). The combined organic extracts were washed with saturated brine, dried over magnesium sulfate, filtered and concentrated. MS 299.2 (M+1).
WORKUP
后处理
- concentrationthe solution was concentrated
- customazeotroped with toluene (2×)
- additionSaturated aqueous sodium bicarbonate solution was added
- extractionthe mixture was extracted with dichloromethane (3×)
- washThe combined organic extracts were washed with saturated brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated