HRID848722

反应详情

EQUATION

反应方程式

HRID 848722 的结构方程式

PROCEDURE

实验过程

Phenyl 4-pyridinyl ketone oxime (5.4 g) was stirred in 50 ml of dimethyl formamide containing 1.5 g of a 50% dispersion of sodium hydride in oil, for 0.5 hours at room temperature. After the hydrogen evolution was completed, chloroacetonitrile (2.5 g) was added. The reaction mixture was stirred for 1 hour. The greater part of the dimethyl formamide was evaporated at reduced pressure, and then the residue was treated with ether and water. The ether layer was separated and dried over magnesium sulphate. The product was recrystallized from a mixture of ether and petroleum ether (40°-60° C.), yielding pure phenyl 4-pyridinyl ketone, O-cyanomethyl oxime (4.9 g, m.p. 101.5°-103° C.).

WORKUP

后处理

  1. customThe greater part of the dimethyl formamide was evaporated at reduced pressure
  2. additionthe residue was treated with ether and water
  3. customThe ether layer was separated
  4. dry with materialdried over magnesium sulphate
  5. customThe product was recrystallized from a mixture of ether and petroleum ether (40°-60° C.)