HRID1604319

反应详情

EQUATION

反应方程式

HRID 1604319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 30 ml of acetonitrile was suspended 3.5 g of 1-benzylidene-2-[4-(4-chloro-α-cyanobenzyl)-3,5-dichlorophenyl]-4-(2,2-dimethoxyethyl)semicarbazide produced in Working Example 2. To the suspension was added 0.7 g of 35% hydrochloric acid, and the reaction was allowed to proceed for one hour at room temperature. After completion of the reaction, the reaction mixture was cooled for 30 minutes at temperatures ranging from 0 to 10° C., then resulting crystalline precipitate was collected by filtration to afford 2.3 g of the titled compound as colorless crystals, m.p. 166-167° C.

WORKUP

后处理

  1. customproduced in Working Example 2
  2. customAfter completion of the reaction
  3. temperaturethe reaction mixture was cooled for 30 minutes at temperatures
  4. customranging from 0 to 10° C.
  5. filtrationresulting crystalline precipitate was collected by filtration