反应详情

Ethyl 3-{[[2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzyl]-(5-hydroxy-pyrimidin-2-yl)-amino]-methyl}-5-trifluoromethyl-benzonitrile (250 mg) and 4-bromobutyrate (76.9 μl) is dissolved in N,N-dimethylformamide (3.7 ml) and thereto is added potassium carbonate (74 mg) and the mixture is stirred at room temperature overnight. Thereto are added ethyl acetate and a saturated brine, and the mixture is separated, and the organic layer is washed with a saturated brine, dried and concentrated under reduced pressure. The resulting residue is purified by NH-silica gel column chromatography (hexane:ethyl acetate=8:1) to give ethyl 4-(2-{(3-cyano-5-trifluoromethyl-benzyl)-[2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzyl]-amino}-pyrimidin-5-yloxy)-butyrate (220 mg). MS (m/z): 678 [M+H]+

1. customa saturated brine, and the mixture is separated
2. washthe organic layer is washed with a saturated brine
3. customdried
4. concentrationconcentrated under reduced pressure
5. customThe resulting residue is purified by NH-silica gel column chromatography (hexane:ethyl acetate=8:1)