HRID1191926
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
CONDITIONS
反应条件
- 温度
- -78 °C
PROCEDURE
实验过程
To a solution of 6-(trifluoromethyl)-1H-indene (1.1 g, 6 mmol) in anhydrous dichloromethane (80 mL) at −78° C. was added a 5.5 M solution of tert-butyl hydroperoxide in n-decane (1.3 mL) followed by titanium tetrachloride (0.79 mL, 7.2 mmol). After being stirred at −78° C. for 1 h, the resulting brown solution was quenched with a mixture of Et2O/saturated Na2SO3 solution. The mixture was stirred at ambient temperature for 1 h to give a colorless solution. The organic layer was separated and washed with brine, dried over MgSO4 and concentrated to give the crude product (1.2 g) as a solid. LC/MS calculated for C10H2F3O: (M+H)+ 201. found 201.0.
WORKUP
后处理
- customthe resulting brown solution was quenched with a mixture of Et2O/saturated Na2SO3 solution
- stirringThe mixture was stirred at ambient temperature for 1 h
- customto give a colorless solution
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated