反应详情

(3,5-Bis-trifluoromethyl-benzyl)-(5′-isopropyl-2′-methoxy-4-trifluoromethyl-biphenyl-2-ylmethyl)-amine (3.0 g) is dissolved in toluene (20 ml) and thereto are added 5-bromo-2-chloropyrimidine (1.6 g) and N,N-diisopropylethylamine (1.4 ml) and the mixture is heated under reflux 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=40:1) to give (3,5-bis-trifluoromethyl-benzyl)-(5-bromo-pyrimidin-2-yl)-(5′-isopropyl-2′-methoxy-4-trifluoromethyl-biphenyl-2-ylmethyl)-amine (2.6 g). MS (m/z): 708/706 [M+H]+

1. temperaturethe mixture is heated
2. temperatureunder reflux overnight
3. extractionthe mixture is extracted with ethyl acetate
4. washThe organic layer is washed with a saturated brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=40:1)