HRID49903
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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
850 mg (3.57 mmol) 4-(4-pyrimidinylmethyl)-1(2H)-phthalazinone in 15 ml acetonitrile is mixed with 1.78 ml (7.14 mmol) 4N HCl solution in dioxane and finally with 1.14 ml (12.5 mmol) phosphoryl chloride. After stirring for 36 h at 50° C., the red suspension is filtered and washed with acetonitrile: FAB MS (M−H)+=255. Further product is obtainable from the evaporated filtrate by distribution between dichloromethane and sat. NaHCO3 solution.
WORKUP
后处理
- filtrationthe red suspension is filtered
- washwashed with acetonitrile