HRID1060585

反应详情

EQUATION

反应方程式

HRID 1060585 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Hydrazine hydrate (0.81 ml, 0.84 g, 16.8 mmoles) was added to a solution under N2 of 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (2 g, 5.6 mmoles), obtained as described in example 13, in ethanol (30 ml), and the mixture was kept under reflux for 24 hours, then cooled in ice and the resultant precipitate was filtered, washed with ethanol and ethyl ether and dried under vacuum at 50° C. to give 2.14 g of the title compound (stoichiometric yield). m.p.: 297-299° C.

WORKUP

后处理

  1. customobtained
  2. temperatureunder reflux for 24 hours
  3. temperaturecooled in ice
  4. filtrationthe resultant precipitate was filtered
  5. washwashed with ethanol and ethyl ether
  6. customdried under vacuum at 50° C.