HRID1071547

反应详情

EQUATION

反应方程式

HRID 1071547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound was prepared by the method of Example 1 using 3.00 g of 2-mercapto-5-ethoxybenzimidazole instead of 2-mercaptobenzimidazole and 2.76 g of 2-(chloromethyl)aniline hydrochloride instead of 2-(chloromethyl)-N,N-dimethylaniline in 250 ml of isopropyl alcohol. The basic extraction used 5% sodium hydroxide instead of sodium carbonate. Crystallization during concentration of the dichloromethane extract gave 2.60 g of the title compound as the monohydrate: m.p. 87-89° C. Analysis. Calc'd. for C16H17N3OS*H2O: C, 63.76; H, 5.68; N, 13.94; S, 10.64. Found: C, 63,65; H, 5.74; N, 13.89; S, 10.89.

WORKUP

后处理

  1. extractionThe basic extraction
  2. customCrystallization during concentration of the dichloromethane
  3. extractionextract