HRID464002

反应详情

EQUATION

反应方程式

HRID 464002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 1N solution of sodium hydroxide (80 ml) was added dropwise to a solution of 7.3 g of diethyl N-(p-chlorobenzoyl)-2-(2-cyanoethyl)aminomalonate in methanol (60 ml) at 0°-5° C., and the resulting mixture was stirred at room temperature for 16 hours. The reaction mixture was then concentrated under reduced pressure to a volume of 80 ml, and 60 ml of ethanol were added to the concentrate. The precipitate was filtered off, washed with 50 ml of ethanol and dried for 16 hours in vacuo, to afford 6.0 g of the desired disodium salt (a) as a colourless powder melting at 254°-255° C. (with decomposition).

WORKUP

后处理

  1. concentrationThe reaction mixture was then concentrated under reduced pressure to a volume of 80 ml, and 60 ml of ethanol
  2. additionwere added to the concentrate
  3. filtrationThe precipitate was filtered off
  4. washwashed with 50 ml of ethanol
  5. customdried for 16 hours in vacuo