HRID1263029

反应详情

EQUATION

反应方程式

HRID 1263029 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 737 mg of ethyl 4-bromo-6,6,6-trichloro-2,3,3-trimethylhexanoate in 20 ml of anhydrous tetrahydrofuran was cooled to 0°. To the cold solution was added 163 mg of sodium ethoxide and the mixture was stirred for 5 hours. The cooled mixture was poured into cold 1N hydrochloric acid and extracted with diethyl ether. The ether extract was washed successively with water, saturated aqueous sodium bicarbonate and aqueous sodium chloride, then dried over magnesium sulfate. The dried ether extract was distilled to give 430 mg (75% yield) of ethyl 6,6,6-trichloro-2,3,3-trimethyl-4-hexenoate, b.p. 92°-95°/0.2 mm.

WORKUP

后处理

  1. extractionextracted with diethyl ether
  2. extractionThe ether extract
  3. washwas washed successively with water, saturated aqueous sodium bicarbonate and aqueous sodium chloride
  4. dry with materialdried over magnesium sulfate
  5. extractionThe dried ether extract
  6. distillationwas distilled