HRID385708

反应详情

EQUATION

反应方程式

HRID 385708 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 cooled (−78° C.) solution of 2-(4-bromo-2,6-difluorophenyl)vinyl methyl ether (45 g, 0.18 mol) in methyl tert-butyl ether (300 mL) was added n-BuLi (75 mL of 2.5M in hexanes, 0.19 mol), and the mixture was stirred at −78° C. for one hour. A solution of acetone (13.6 g, 0.24 mol) in methyl tert-butyl ether (100 mL) was added dropwise to the reaction mixture and the resulting solution was stirred at −78° C. for two hours. Water (90 ml) was added to quench the reaction. The resulting biphasic mixture was extracted with ethyl acetate (2×). The organic layers were dried and concentrated in vacuo. Purification via flash chromatography afforded the title compound.

WORKUP

后处理

  1. stirringthe resulting solution was stirred at −78° C. for two hours
  2. customto quench
  3. customthe reaction
  4. extractionThe resulting biphasic mixture was extracted with ethyl acetate (2×)
  5. customThe organic layers were dried
  6. concentrationconcentrated in vacuo
  7. customPurification via flash chromatography