HRID1974616

反应详情

EQUATION

反应方程式

HRID 1974616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of lithium aluminium hydride (44.1 g, 1.16 mmol) in absolute ether (700 ml) is treated dropwise with a solution of 3'-chloro-4'-fluoroacetanilide (BE Patent No. 891537; 109 g, 0.576 mol) in absolute THF (350 ml). The suspension obtained is stirred for 2 hours, then cooled to 0° and treated with a Rochelle salt solution (350 ml). The crystals obtained are filtered off and washed with ether. The organic solution is dried over magnesium sulphate and the solvent is distilled off under reduced pressure. There are obtained 97.5 g (97.5%) of 3-chloro-N-ethyl-4-fluoroaniline as an amorphous material.

WORKUP

后处理

  1. customThe suspension obtained
  2. temperaturecooled to 0°
  3. customThe crystals obtained
  4. filtrationare filtered off
  5. washwashed with ether
  6. dry with materialThe organic solution is dried over magnesium sulphate
  7. distillationthe solvent is distilled off under reduced pressure