HRID35296

反应详情

EQUATION

反应方程式

HRID 35296 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 20 parts of 2-chloroethanol, 3 parts of sulfuric acid and 16 parts of benzene was heated on a water-bath. Then there were added dropwise 35 parts of 4-fluoro-α-(4-fluorophenyl)benzenemethanol dissolved in 32 parts of benzene. After the addition was complete, the whole was stirred and refluxed for 4 hours. After cooling the reaction mixture was poured into water. The benzene layer was separated, dried over calcium chloride and evaporated. The residue was distilled in vacuo, yielding 35 parts of 1,1'-[(2-chloroethoxy)methylene]bis[4-fluorobenzene]; bp. 164°-166° C. at 1.5 mm. pressure; nD20 : 1.5462; d2020 : 1.2290 (intermediate 1).

WORKUP

后处理

  1. temperaturewas heated on a water-bath
  2. additionAfter the addition
  3. temperaturerefluxed for 4 hours
  4. temperatureAfter cooling the reaction mixture
  5. customThe benzene layer was separated
  6. dry with materialdried over calcium chloride
  7. customevaporated
  8. distillationThe residue was distilled in vacuo