HRID1282434

反应详情

EQUATION

反应方程式

HRID 1282434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

An amount (13.9 g) of 1-fluoro-2-fluoromethyl-3-butyn-2-yl 4-trifluoromethylphenyl ether was dissolved in a solvent consisting of a mixture of tert-butyl methyl ether (100 ml) and tert-butyl alcohol (150 ml). To the solution under cooling with ice, potassium tert-butoxide (7.1 g) was added under a nitrogen atmosphere; after stirring for a while, bromine (3 ml) was added dropwise. After the end of the dropwise addition, the mixture was stirred for 30 minutes under stirring with ice. Hexane was added to the reaction mixture, which was then washed with water and a saturated aqueous solution of sodium chloride. The mixture was dried with anhydrous sodium sulfate and concentrated under reduced pressure to give the titled compound (18.1 g).

WORKUP

后处理

  1. additionwas added under a nitrogen atmosphere
  2. additionwas added dropwise
  3. additionAfter the end of the dropwise addition
  4. stirringunder stirring with ice
  5. washwas then washed with water
  6. dry with materialThe mixture was dried with anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure