反应详情

温度

50 °C

2-[(3,5-Bis-trifluoromethyl-benzyl)-(5′-isopropyl-2′-methoxy-4-trifluoromethyl-biphenyl-2-ylmethyl)-amino]-pyrimidin-5-ol (300 mg) is dissolved in tetrahydrofuran (2 mL), and thereto are added 2-(methylthio)ethanol (162 μl) and triphenylphosphine (488 mg), and thereto is added dropwise a 40% diethyl azodicarboxylate/toluene solution (424 μl) under water-cooling, and the mixture is stirred at 50° C. overnight. Further thereto are added 2-(methylthio)ethanol (243 μl) and triphenylphosphine (244 mg), and thereto is added dropwise diisopropyl azodicarboxylate (361 μl) under water-cooling, and the mixture is stirred at 60° C. for 2 hours. To the reaction mixture is added a saturated brine, and the mixture is extracted with ethyl acetate. The organic layer is washed with a saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=99:1→9:1) to give (3,5-bis-trifluoromethyl-benzyl)-(5′-isopropyl-2′-methoxy-4-trifluoromethyl-biphenyl-2-ylmethyl)-[5-(2-methylsulfanyl-ethoxy)-pyrimidin-2-yl]-amine (300 mg). MS (m/z): 718 [M+H]+

1. temperaturecooling
2. temperaturecooling
3. stirringthe mixture is stirred at 60° C. for 2 hours
4. extractionthe mixture is extracted with ethyl acetate
5. washThe organic layer is washed with a saturated brine
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=99:1→9:1)