HRID262144

反应详情

EQUATION

反应方程式

HRID 262144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Sodium hydride (0.93 g, 80% dispersion in oil) was added to a solution of 2,2-dimethyl-4-(3-trifluoromethylphenyl)chroman-7-ol (containing 1 mole of carbon tetrachloride of crystallisation) (7.5 g) in dimethylformamide (25 ml). Chloroacetonitrile (1.76 g) was added and the mixture heated at 60° C. for 3 hours. The solvent was removed under reduced pressure and the resulting oil was poured into water. The aqueous solution was extracted with ether and the etheeal extracts were dried (MgSO4) and evaporated under reduced pressure to yield an oil. Chromatography on alumina with ether--petrol (40°-60° C.), 1:3 as eluate gave the title compound which crystallised on standing.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. additionthe resulting oil was poured into water
  3. extractionThe aqueous solution was extracted with ether
  4. dry with materialthe etheeal extracts were dried (MgSO4)
  5. customevaporated under reduced pressure
  6. customto yield an oil