HRID133131
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
To a solution of tert-butyl (3R,6S)-6-(2,3-difluorophenyl)-2-oxo-1-(2,2,2-trifluoroethyl)azepan-3-ylcarbamate from Step F (135 mg, 0.320 mmol) in CH2Cl2 (5 mL) was added CF3CO2H (2.5 mL). After 30 min, the solution was concentrated in vacuo and azeotroped with toluene (2×). Saturated aqueous NaHCO3 was added and the mixture was extracted with CH2Cl2 (3×). The combined organic extracts were washed with brine, dried over MgSO4, filtered and concentrated in vacuo to give the title compound. MS: m/z=323 (M+1).
WORKUP
后处理
- concentrationthe solution was concentrated in vacuo
- customazeotroped with toluene (2×)
- additionSaturated aqueous NaHCO3 was added
- extractionthe mixture was extracted with CH2Cl2 (3×)
- washThe combined organic extracts were washed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo