HRID1733697

反应详情

EQUATION

反应方程式

HRID 1733697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In ethyl acetate (50 ml) are dissolved ethyl 2-hydroxyimino-2-cyanoacetate (7.1 g) and triethylamine (7.0 ml). To the solution is added p-toluenesulfonyl chloride (9.5 g) with stirring under ice-cooling, and the mixture is stirred for 2 hours and allowed to stand overnight. The reaction mixture is filtered and the filtrate is concentrated. To the residue is added cyclohexane and the resulting crystals are separated by filtration and dried to give ethyl 2-(p-toluenesulfonyloxyimino)-2-cyanoacetate (13.9 g), melting point: 84°-87° C.

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture is stirred for 2 hours
  3. filtrationThe reaction mixture is filtered
  4. concentrationthe filtrate is concentrated
  5. additionTo the residue is added cyclohexane
  6. customthe resulting crystals are separated by filtration
  7. customdried