HRID1792491

反应详情

EQUATION

反应方程式

HRID 1792491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

14.4 mL chlorosulfonic acid and 14.42 mL thionyl chloride were added to 7.78 g of 6-bromo-4-(2-thienyl)quinazoline (compound in Production Example 96) under ice-cooling in a stream of nitrogen, and the mixture was heated at 60° C. for 16 hours, then poured into iced water, neutralized by adding a sodium bicarbonate solution and extracted with dichloromethane. The organic layer was dried over anhydrous sodium sulfate. The residue was recrystallized from ether/hexane, to give 2.47 g of the title compound (pale skin-colored crystals).

WORKUP

后处理

  1. temperaturecooling in a stream of nitrogen
  2. extractionextracted with dichloromethane
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. customThe residue was recrystallized from ether/hexane