HRID1970189

反应详情

EQUATION

反应方程式

HRID 1970189 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe resulting content was maintained at −78° C. for 3 hours
  2. temperatureslowly warmed up to RT overnight
  3. customThe reaction mixture was then partitioned between ethyl acetate and water
  4. washThe ethyl acetate layer was then washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customthe solvent evaporated in vacuo
  8. customto yield a crude oil
  9. customThe crude solid was purified via flash chromatography (15% EtOAc in n-hexane)