反应详情

Tert-butyl 4-[2-(3,5-bis-trifluoromethyl-benzyl-amino)-pyrimidin-5-yloxy]-butyrate (100 mg) is dissolved in DMF (1 ml) and thereto is added sodium hydride (60%) (10.8 mg) under ice-cooling, and the mixture is stirred under ice-cooling for 15 minutes. Thereto is added 1-bromo-2-chloromethyl-4,5-dimethoxybenzene (83.1 mg) and the mixture is stirred under ice-cooling for 1 hour. To the reaction solution are added aqueous ammonium chloride solution and ethyl acetate, and the mixture is separated, and the organic layer is washed with a saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (hexane:ethyl acetate=10:1→14:1) to give tert-butyl 4-{2-[(3,5-bis-trifluoromethyl-benzyl)-(2-bromo-4,5-dimethoxy-benzyl)-amino]-pyrimidin-5-yloxy}-butyrate (116 mg). MS (m/z): 708/710 [M+H]+

1. temperaturecooling
2. temperaturecooling for 15 minutes
3. stirringthe mixture is stirred under ice-
4. temperaturecooling for 1 hour
5. customthe mixture is separated
6. washthe organic layer is washed with a saturated brine
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe residue is purified by silica gel column chromatography (hexane:ethyl acetate=10:1→14:1)