HRID263086

反应详情

EQUATION

反应方程式

HRID 263086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 5.37 g (0.0772 mol) of hydroxylamine hydrochloride and of 7.72 g (0.0772 mol) of potassium bicarbonate in 8 ml of water is added, all at once, to a suspension of 10 g (0.0385 mol) of 4-(4-chlorophenoxy)-phenoxy-acetonitrile prepared as indicated in Example 29a), in 24 ml of n-butanol. The mixture is heated to the reflux temperature for 1 hour, the butanol is driven off, the residue is taken up in water and the insoluble matter is extracted with diethyl ether. The organic phase is washed with water, dried over dry sodium sulphate and evaporated, and the residue obtained is purified by washing with hot diisopropyl ether to give 10 g of brilliant white needles.

WORKUP

后处理

  1. customprepared
  2. temperatureThe mixture is heated to the reflux temperature for 1 hour
  3. extractionthe insoluble matter is extracted with diethyl ether
  4. washThe organic phase is washed with water
  5. dry with materialdried over dry sodium sulphate
  6. customevaporated
  7. customthe residue obtained
  8. customis purified
  9. washby washing with hot diisopropyl ether