HRID2269265
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a stirred solution of Compound 56 (0.22 g, 1.26 mmol) in THF (8 ml) was added n-BuLi (1.69 M in hexane, 0.82 ml, 1.39 mmol) at −78° C. under N2, then warmed up to 0° C., and stirred for 1 h. S-(Trifluoromethyl)dibenzothiophenium trifluoromethane-sulfonate (1.01 g, 2.52 mmol) was added, and stirred for 3 h at 0° C. The mixture was quenched by the addition of NaHCO3 aq., and extracted with CH2Cl2. The combined organic layers were dried over MgSO4, filtered, and concentrated. This was purified by SiO2 chromatography to give Compound 57 (38 mg, 13%) as a colorless oil.
WORKUP
后处理
- stirringstirred for 3 h at 0° C
- customThe mixture was quenched by the addition of NaHCO3 aq.
- extractionextracted with CH2Cl2
- dry with materialThe combined organic layers were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThis was purified by SiO2 chromatography