HRID969734

反应详情

EQUATION

反应方程式

HRID 969734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 11 g of 4-(2,4-difluoro-benzoyl)piperidine-oxime hydrochloride and 25 g of potassium hydroxide in 25 ml of water is heated to boiling with stirring for 2 hours. The reaction mixture is cooled to room temperature and extracted with toluene. The organic phase is dried over anhydrous sodium sulfate and evaporated in vacuo. The residual crude product is recrystallized from petroleum ether. Thus 7.1 g of the title compound are obtained. According to HPLC MS analysis the product contains 5% of 4-{6-[4′-(6′-fluoro-1′,2′-benzisoxazol-3′-yl)-piperidine-1′-yl]-1,2-benzisoxazol-3-yl}-piperidine, as a contamination (compound of the Formula VI).

WORKUP

后处理

  1. temperatureis heated
  2. extractionextracted with toluene
  3. dry with materialThe organic phase is dried over anhydrous sodium sulfate
  4. customevaporated in vacuo
  5. customThe residual crude product is recrystallized from petroleum ether