HRID2398160

反应详情

EQUATION

反应方程式

HRID 2398160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

8.05 Ml. of dimethylcarbamoyl chloride are added dropwise while cooling at about 25° C. in the course of 3 minutes to a solution of 21.5 g. of 2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonamide hydrochloride and 24.5 ml. of triethylamine in 400 ml. of methanol and the mixture is subsequently stirred for a further 15 hours, during which a crystalline precipitate results. By evaporation of the solvent in vacuo and digestion and washing of the crystalline evaporation residue with water, there is obtained 3-dimethylcarbamoyl-2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonamide, m.p. 192°-193° C.

WORKUP

后处理

  1. customresults
  2. customBy evaporation of the solvent in vacuo and digestion
  3. washwashing of the crystalline evaporation residue with water