反应详情

温度

90 °C

(3,5-Bis-trifluoromethyl-benzyl)-(5-bromo-pyrimidin-2-yl)-(5′-isopropyl-2′-methoxy-4-trifluoromethyl-biphenyl-2-ylmethyl)-amine (1.2 g) is dissolved in N,N-dimethylformamide (6 ml) and thereto are added palladium acetate (II) (76 mg), 1,1′-bis(diphenylphosphino)ferrocene (376 mg), ethanol (4.0 ml) and triethylamine (4.8 ml), and the mixture is stirred under carbon monoxide at 90° C. overnight. The reaction solution is allowed to cool to room temperature, and thereto is added water 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=20:1→10:1) to give ethyl 2-[(3,5-bis-trifluoromethyl-benzyl)-(5′-isopropyl-2′-methoxy-4-trifluoromethyl-biphenyl-2-ylmethyl)-amino]-pyrimidine-5-carboxylate (1.1 g). MS (m/z): 700 [M+H]+

1. temperatureto cool to room temperature
2. extractionthe mixture is extracted with ethyl acetate
3. washThe organic layer is washed with a saturated brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=20:1→10:1)