HRID268474

反应详情

EQUATION

反应方程式

HRID 268474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6.6 g. (0.044 mol.) of p-chlorophenylacetonitrile and 20 ml. of dry glyme was added 6.2 g. (0.13 mol.) of sodium hydride (50% in oil). Ethyl 3-cyano-3-phenylpyruvate (9.55 g., 0.044 mol.) was added in portions at -10° and the reaction mixture was stirred at 25° for 12 hours. The mixture was diluted with 150 ml. of water, extracted with ether, acidified with 15 ml. of acetic acid and the solid was collected by filtration to yield 2-(p-chloro-phenyl)-5-phenyl-3,4-dioxoadiponitrile, m.p. 210° (dec.).

WORKUP

后处理

  1. additionThe mixture was diluted with 150 ml
  2. extractionof water, extracted with ether
  3. filtrationof acetic acid and the solid was collected by filtration