反应详情

温度

105 °C

The 7-((S)-2,3-dihydroxypropylamino)-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (281.9 mg, 0.745 mmol) obtained in step A was suspended in diethyl carbonate (2.93 ml), and thereafter, a 28% sodium methoxide-methanol solution (117 μl) was added thereto. The obtained mixture was stirred at 105° C. for 13 hours. Thereafter, diethyl carbonate was distilled away under reduced pressure. The obtained residue was dissolved in methanol (15 ml), and the obtained solution was stirred under heating to reflux for 10 minutes. Thereafter, the reaction solution was concentrated, and a saturated ammonium chloride aqueous solution was then added to the residue, followed by extraction with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and was then concentrated. The obtained residue was purified by silica gel column chromatography (methylene chloride:methanol=40:1 to 20:1), so as to obtain 7-((S)-5-hydroxymethyl-2-oxooxazolidin-3-yl)-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (233.8 mg; yield: 78%).

1. distillationThereafter, diethyl carbonate was distilled away under reduced pressure
2. dissolutionThe obtained residue was dissolved in methanol (15 ml)
3. stirringthe obtained solution was stirred
4. temperatureunder heating
5. temperatureto reflux for 10 minutes
6. concentrationThereafter, the reaction solution was concentrated
7. additiona saturated ammonium chloride aqueous solution was then added to the residue
8. extractionfollowed by extraction with ethyl acetate
9. dry with materialThe extract was dried over anhydrous sodium sulfate
10. concentrationwas then concentrated
11. customThe obtained residue was purified by silica gel column chromatography (methylene chloride:methanol=40:1 to 20:1)