HRID1065845

反应详情

EQUATION

反应方程式

HRID 1065845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

A mixture of 3,6-dichloro-4-carboxy-pyridazine (20 g; 0.103 mole) and 22 ml of 98% hydrazine hydrate in 200 ml of 50% ethanol was refluxed, under stirring, for one hour. After cooling at 5° C., the solid precipitate was collected, washed with 20 ml of anhydrous ethanol. The solid was suspended in 100 ml of water, the mixture was brought to pH 1-2 with 23% HCl, after cooling at 5° C. the solid was filtered, dried under vacuum at 80° C. to give 18.29 g (93.4%) of the title compound, m.p. 198°-201° C.

WORKUP

后处理

  1. temperaturewas refluxed
  2. customthe solid precipitate was collected
  3. washwashed with 20 ml of anhydrous ethanol
  4. temperatureafter cooling at 5° C. the solid
  5. filtrationwas filtered
  6. customdried under vacuum at 80° C.