HRID33977
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
To a solution of 2-(N′-methoxy-N′-methylaminocarbonylmethylamino)-3-methyl-5-naphthalen-2-yl-6-pyridin-4-yl-3H-pyrimidin-4-one (1.46 g, 3.4 mmol) in THF (30 mL) at 0° C. was slowly added benzylmagnesium chloride (Aldrich, 2.5M in THF, 20 mL). After 2 h, water (100 mL) and ethyl acetate (200 mL) were added. The layers were separated. The organic layer was washed with brine (3×80 mL), dried, and evaporated to give the crude product. Column chromatograph purification (silica gel, 1-2% MeOH/CH2Cl2) gave the final product. M+1=491.2.
WORKUP
后处理
- customat 0° C.
- customThe layers were separated
- washThe organic layer was washed with brine (3×80 mL)
- customdried
- customevaporated
- customto give the crude product
- customColumn chromatograph purification (silica gel, 1-2% MeOH/CH2Cl2)