HRID647807

反应详情

EQUATION

反应方程式

HRID 647807 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4.45 g (32.0 millimoles) of 1-chlorocyclopropanecarboxylic acid chloride in 20 ml of absolute tetrahydrofuran is added dropwise to a stirred suspension of 5.0 g (26.4 millimoles) of 6-(p-aminophenyl)-4,5-dihydro-3(2H)-pyridazinone in 100 ml of absolute tetrahydrofuran. The mixture is then stirred for 20 hours at room temperature followed by 1 hour under reflux. The product is filtered off at 10° C., washed first with tetrahydrofuran and then with water, and recrystallized from dimethylformamide/water. 6.3 g (82% of theory) of 6-[p-(1-chlorocyclopropylcarbonylamino)-phenyl]-4,5-dihydro-3(2H)-pyridazinone are isolated as colorless crystals, of melting point 231°-232° C.

WORKUP

后处理

  1. waitfollowed by 1 hour
  2. temperatureunder reflux
  3. filtrationThe product is filtered off at 10° C.
  4. washwashed first with tetrahydrofuran
  5. customwith water, and recrystallized from dimethylformamide/water