反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of phenol (94 mg, 1 mmol) in dioxane (5 ml) was added sodium hydride (40 mg of a 60% dispersion in mineral oil, 1.0 mmol). The mixture was stirred at room temperature for 10 minutes. Then, 4-chloro-6-(4-fluorophenyl)-pyrido[3,2-d]pyrimidine (52 mg, 0.2 mmol) was added to this solution. The resulting mixture was stirred at room temperature for another 30 minutes. After concentration under reduced pressure, the residue was purified by silica gel flash chromatography, the mobile phase being a mixture of methanol and dichloromethane, in a volume ratio of 1:60, yielding the title compound (60 mg, yield 95%) as a white solid which was characterised by its mass spectrum as follows: MS (m/z): 318 ([M+H]+, 100).
WORKUP
后处理
- stirringThe resulting mixture was stirred at room temperature for another 30 minutes
- concentrationAfter concentration under reduced pressure
- customthe residue was purified by silica gel flash chromatography
- additiona mixture of methanol and dichloromethane