反应详情

温度

40 °C

Ethyl 4-(2-{(3-cyano-5-trifluoromethyl-benzyl)-[2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzyl]-amino}-pyrimidin-5-yloxy)-butyrate (240 mg) is dissolved in tetrahydrofuran (2.6 ml), and thereto is added 1N-aqueous sodium hydroxide solution (2.6 ml) and the mixture is stirred at 40° C. for additional 30 minutes and warmed to 50° C. and stirred for 3 hours. Thereto is added a 2N-aqueous sodium hydroxide solution (650 μl) and the mixture is stirred at 60° C. for 20 minutes. The reaction solution is cooled to room temperature and thereto are added ethyl acetate and a 1N-hydrochloric acid, and the mixture is separated, and the organic layer is washed with a saturated brine, dried over sodium sulfate and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (chloroform:methanol=19:1) to give 4-(2-{(3-cyano-5-trifluoromethyl-benzyl)-[2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzyl]-amino}-pyrimidin-5-yloxy)-butyric acid (189 mg). MS (m/z): 650 [M+H]+

1. temperaturewarmed to 50° C.
2. stirringstirred for 3 hours
3. stirringthe mixture is stirred at 60° C. for 20 minutes
4. temperatureThe reaction solution is cooled to room temperature
5. customa 1N-hydrochloric acid, and the mixture is separated
6. washthe organic layer is washed with a saturated brine
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe resulting residue is purified by silica gel column chromatography (chloroform:methanol=19:1)