HRID1060584
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customobtained
- temperaturethe mixture was heated
- temperatureunder reflux
- concentrationAfter 3 hours the solution was concentrated
- customdried
- concentrationconcentrated