HRID1253599

反应详情

EQUATION

反应方程式

HRID 1253599 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

The mixture of 0.45 g (1.5 mmol) of 6-chloro-2-phenyl-3-(pyridazin-4-yl)imidazo[1,2-b]pyridazine and 0.38 g (2.9 mmol) of 1-isopropylpiperazine in 6 ml of pentanol is heated in a sealed tube at 150° C. for 2 days. The mixture is cooled and poured into a 1N aqueous solution of hydrochloric acid. This solution is washed with diethyl ether and then basified using an aqueous solution of sodium hydroxide. The product is finally extracted with dichloromethane, and the organic phase is dried over sodium sulfate, filtered and concentrated under reduced pressure. A brown oil is obtained, which is chromatographed on silica gel, elution being carried out with a mixture of aqueous ammonia, methanol and dichloromethane (0.4/4/96), to give 0.50 g of a solid.

WORKUP

后处理

  1. temperatureThe mixture is cooled
  2. washThis solution is washed with diethyl ether
  3. extractionThe product is finally extracted with dichloromethane
  4. dry with materialthe organic phase is dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customA brown oil is obtained
  8. customwhich is chromatographed on silica gel, elution
  9. additionbeing carried out with a mixture of aqueous ammonia, methanol and dichloromethane (0.4/4/96)