HRID1637632

反应详情

EQUATION

反应方程式

HRID 1637632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 6-[3-(2-chloromethyl-3-methylpyridin-4-ylsulfanyl)propylsulfanyl]-3-nitroimidazo[1,2-b]pyridazine (1.23 g, 3.0 mmol), 2-mercaptopyrimidine (330 mg, 2.9 mmol) and triethylamine (335 mg, 3.3 mmol) in isopropanol (100 ml) is heated under reflux for 4.5 h. After cooling, the suspension is stirred at room temperature for a further 18 h and then at 0° C. for 0.5 h. The precipitate is filtered off, washed with isopropanol and dried at 40° C. in vacuo. The crystalline solid is then suspended in water (50 ml) and sodium carbonate solution (10 ml). After filtration and drying in vacuo at 40° C., the title compound is isolated as a pale beige solid. Yield 1.40 g (93%), m.p. 143-147° C.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 4.5 h
  3. temperatureAfter cooling
  4. waitat 0° C. for 0.5 h
  5. filtrationThe precipitate is filtered off
  6. washwashed with isopropanol
  7. customdried at 40° C. in vacuo
  8. filtrationAfter filtration
  9. customdrying in vacuo at 40° C.