HRID1110329

反应详情

EQUATION

反应方程式

HRID 1110329 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11.18 g (40 millimoles) of 6-[p-(3-chloropropionylamino)-phenyl]-4,5-dihydro-3(2H)-pyridazinone in 250 ml of ethanol were initially taken and 26.5 g (220 millimoles) of 2-phenylethylamine were added dropwise, after which the mixture was refluxed for 6 hours. Insoluble material was filtered off, the solvent was stripped off and the mother liquor was then crystallized by adding acetone. The product was recrystallized twice from methanol to give 5.3 g of 6-{p-[3-(2-phenylethylamino)-propionylamino]-phenyl}-4,5-dihydro-3(2H)-pyridazinone.HCl of melting point 269°-270° C.

WORKUP

后处理

  1. temperatureafter which the mixture was refluxed for 6 hours
  2. filtrationInsoluble material was filtered off
  3. customthe mother liquor was then crystallized
  4. additionby adding acetone
  5. customThe product was recrystallized twice from methanol