反应详情

2-[(2-Benzyloxy-5-trifluoromethyl-benzyl)-(3,5-bis-trifluoromethyl-benzyl)-amino]-pyrimidin-5-ol (1.33 g) is dissolved in tetrahydrofuran (20 ml), and thereto are added 2-methylsulfanyl-ethanol (290 μl), triphenylphosphine (870 mg) and 40% diethyl azodicarboxylate/toluene solution (1.5 ml) and the mixture is stirred at room temperature for 45 minutes. To the reaction solution are added water 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 resulting residue is purified by NH-silica gel column chromatography (hexane:ethyl acetate=99:1→19:1) to give (2-benzyloxy-5-trifluoromethyl-benzyl)-(3,5-bis-trifluoromethyl-benzyl)-[5-(2-methylsulfanyl-ethoxy)-pyrimidin-2-yl]-amine (1.21 g). MS (m/z): 676 [M+H]+

1. customthe mixture is separated
2. washthe organic layer is washed with a saturated brine
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe resulting residue is purified by NH-silica gel column chromatography (hexane:ethyl acetate=99:1→19:1)