HRID1833851

反应详情

EQUATION

反应方程式

HRID 1833851 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Thionyl chloride (100 ml.) was added to a solution of 1-(2-fluorophenyl)ethanol [described by McCall, J.A.C.S. 74, 4809 (1952)] (105 g.) in dry chloroform (200 ml.). After the vigorous initial reaction had subsided, the solution was heated at reflux on a steam bath for 30 minutes. The excess of thionyl chloride was removed by repeated co-distillation with dry toluene and the residue was diluted with diethyl ether, washed with water (2 × 100 ml.), dried over sodium sulphate, filtered and evaporated to a yellow liquid, which was distilled to give 1-(2-fluorophenyl)ethyl chloride (73.2 g.), b.p. 70°-75° C./20 mm.Hg, as a pale yellow oil.

WORKUP

后处理

  1. customAfter the vigorous initial reaction
  2. temperaturethe solution was heated
  3. temperatureat reflux on a steam bath for 30 minutes
  4. customThe excess of thionyl chloride was removed
  5. additionthe residue was diluted with diethyl ether
  6. washwashed with water (2 × 100 ml.)
  7. dry with materialdried over sodium sulphate
  8. filtrationfiltered
  9. customevaporated to a yellow liquid, which
  10. distillationwas distilled