HRID1970189
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 4-Bromo-1-methyl-2-trifluoromethyl-benzene (3.4 g, 14.2 mmol) in THF was added n-BuLi at −78° C. After the reaction mixture was stirred at −78° C. for 30 minutes, dry acetone was slowly added. The resulting content was maintained at −78° C. for 3 hours and slowly warmed up to RT overnight. The reaction mixture was then partitioned between ethyl acetate and water. The ethyl acetate layer was then washed with brine, dried over Na2SO4, filtered, and the solvent evaporated in vacuo to yield a crude oil. The crude solid was purified via flash chromatography (15% EtOAc in n-hexane) yielded the title compound as an oil (2.7 g, 86%)
WORKUP
后处理
- temperatureThe resulting content was maintained at −78° C. for 3 hours
- temperatureslowly warmed up to RT overnight
- customThe reaction mixture was then partitioned between ethyl acetate and water
- washThe ethyl acetate layer was then washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- customthe solvent evaporated in vacuo
- customto yield a crude oil
- customThe crude solid was purified via flash chromatography (15% EtOAc in n-hexane)