HRID1704000

反应详情

EQUATION

反应方程式

HRID 1704000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.1 g (0.005 mole) of 8-chloro-6-(2-chlorophenyl)-1-methylthio-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid methyl ester and 20 ml of a 28% solution of methylamine in ethanol was heated at 130° in a steel bomb for 18 hrs. The contents of the bomb were evaporated at reduced pressure to give a tan solid. Recrystallization from ethanol gave off-white prisms with mp 224°-227°. Uv λ max 218 mμ (ε=51,400) infl 245 (26,000) sh 275 (12,000); ir (KBr) 3410 cm-1 (NH) 1668, 1527 (CON).

WORKUP

后处理

  1. customThe contents of the bomb were evaporated at reduced pressure
  2. customto give a tan solid
  3. customRecrystallization from ethanol
  4. customgave off-white prisms with mp 224°-227°