HRID463655

反应详情

EQUATION

反应方程式

HRID 463655 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.9 g (57.0 millimoles) of cyanoacetyl chloride were added dropwise to 6.0 g (31.7 millimoles) of 6-(p-aminophenyl)-4,5-dihydro-3(2H)-pyridazinone in 150 ml of absolute tetrahydrofuran at room temperature, while stirring. After the addition was complete, stirring was continued for a further 10 minutes at 50° C. The product was filtered off under suction at 10° C., washed first with tetrahydrofuran and then with water and recrystallized from dimethylformamide/water. 4.4 g (54%) of 6-[p-(cyanoacetylamino)-phenyl]-4.5,-dihydro-3(2H)-pyridazinone were obtained as pale beige crystals. Mp.: 270° C. (decomposition).

WORKUP

后处理

  1. additionAfter the addition
  2. stirringstirring
  3. filtrationThe product was filtered off under suction at 10° C.
  4. washwashed first with tetrahydrofuran
  5. customwith water and recrystallized from dimethylformamide/water