HRID1039368

反应详情

EQUATION

反应方程式

HRID 1039368 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

2-Hydroxymethyl-5,7-dimethyl-3-(2-methylsulfamoylphenyl)-4-oxo-3,4-dihydro-quinazoline-6-carboxylic acid: 2-Benzyloxymethyl-5,7-dimethyl-3-(2-methylsulfamoyl-phenyl)-4-oxo-3,4-dihydro-quinazoline-6-carboxylic acid ethyl ester (3 g, 5.6 mmol) is dissolved in 47% hydrobromic acid. The reaction mixture is stirred at 80° C. overnight, then at 90° C. for 5 h, then at 95° C. for a further 5 h. The reaction mixture is evaporated in vacuo to give a brown solid, which is suspended in diethyl ether/dichloromethane and stirred overnight. Filtration, followed by washing with dichloromethane then ether and drying in vacuo provides the title compound as a sandy brown solid.

WORKUP

后处理

  1. waitat 90° C. for 5 h
  2. waitat 95° C. for a further 5 h
  3. customThe reaction mixture is evaporated in vacuo
  4. customto give a brown solid, which
  5. stirringstirred overnight
  6. filtrationFiltration
  7. washby washing with dichloromethane
  8. dry with materialether and drying in vacuo