HRID568667

反应详情

EQUATION

反应方程式

HRID 568667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-chloro-2'-fluoro-2-hydroxy-4-methoxybenzophenone (24.6 g) is refluxed for 18 hours in 300 ml of pyridine containing 12.2 g of hydroxylamine hydrochloride. The reaction mixture is concentrated under reduced pressure and is distributed between ether and 5% HCl. The organic phase is dried and evaporated and the resulting crystalline product fused at 205° C. for 45 minutes. The product is cooled and recrystallized from toluene to give E-3-chloro-2'-fluoro-2-hydroxy-4-methoxybenzophenone oxime, mp 184°-186° C.

WORKUP

后处理

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. customThe organic phase is dried
  3. customevaporated
  4. temperatureThe product is cooled
  5. customrecrystallized from toluene