HRID1060584

反应详情

EQUATION

反应方程式

HRID 1060584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

POCl3 (22.2 ml, 230 mmoles) was added to a suspension of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-2H-phthalazin-1-one (10 g, 25.5 mmoles), obtained as described in example 12, in acetonitrile (300 ml) and the mixture was heated under reflux. After 3 hours the solution was concentrated, taken up with CH2Cl2, with water, and the pH was brought to 7-8 with Na2CO3. The organic phases were decoloured with charcoal, dried and concentrated to give 10 g of the title compound (stoichiometric yield).

WORKUP

后处理

  1. customobtained
  2. temperaturethe mixture was heated
  3. temperatureunder reflux
  4. concentrationAfter 3 hours the solution was concentrated
  5. customdried
  6. concentrationconcentrated