HRID2268857

反应详情

EQUATION

反应方程式

HRID 2268857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-2H-phthalazin-1-one (10 g, 25.5 mmoles), prepared as described in example 38, in acetonitrile (300 ml), was added with POCl3 (22.2 ml, 230 mmoles) and the mixture was refluxed. After 3 hours, the solution was concentrated, taken up in CH2Cl2, in water, and the pH was brought to 7-8 by Na2CO3. The organic phases were discoloured with charcoal, anhydrified and concentrated to give 10 g of the title compound (stoichiometric yield). m.p.: 156-166° C.

WORKUP

后处理

  1. customprepared
  2. temperaturethe mixture was refluxed
  3. concentrationthe solution was concentrated
  4. concentrationconcentrated