反应详情

To a solution of 2-(N′-methoxy-N′-methylaminocarbonylmethylamino)-3-methyl-5-naphthalen-2-yl-6-pyridin-4-yl-3H-pyrimidin-4-one (400 mg, 0.93 mmol) in THF (10 mL) at 0° C. was slowly added 3-methoxybenzylmagnesium chloride (Rieke Metal, 0.25 M in THF, 20 mL). After 3 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 crude product. Column chromatograph purification (silica gel, 1-2% MeOH/CH2Cl2) gave the product as a solid. M+1=491.2.

1. customat 0° C.
2. customThe layers were separated
3. washThe organic layer was washed with brine (3×80 mL)
4. customdried
5. customevaporated
6. customto give crude product
7. customColumn chromatograph purification (silica gel, 1-2% MeOH/CH2Cl2)