HRID364952

反应详情

EQUATION

反应方程式

HRID 364952 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

16.0 g. of 2,6-dichlorobenzoylisocyanate are added in small portions to a solution of 11.66 g. of p-chloroanilino-acetonitrile in 100 ml. of dry benzene with moderate cooling. After some time a substance crystallizes out, which after about 12 hours is drawn off and washed with benzene. After drying the weight is 25.25 g, i.e. 93.7% the melting point being 185° C., with spontaneous decomposition on the Kofler heating bench. Thin-layer chromatography (solvent either ethylacetate or chloroform) shows that the substance is pure, however, if desired, it may be recrystallized from 250 ml. of benzene with a yield of 80%.

WORKUP

后处理

  1. customAfter some time a substance crystallizes out
  2. washwashed with benzene
  3. customAfter drying the weight
  4. custombeing 185° C., with spontaneous decomposition on the Kofler
  5. temperatureheating bench
  6. customit may be recrystallized from 250 ml