反应详情

温度

70 °C

Dimethylsulfoxide (DMSO) (3 ml), acetic anhydride (1.5 ml), and acetic acid (1.5 ml) were added to tolvaptan (1.0 g, 2.2 mmol), and the mixture was stirred at 70° C. for 4 hours. Water and 1N aqueous sodium hydroxide solution were added to the reaction mixture, and the mixture was extracted with ethyl acetate, washed with an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate. After filtration and concentration under reduced pressure, the residue was purified by silica gel flash chromatography (n-hexane:ethyl acetate=80:20→20:80). The purified product was concentrated under reduced pressure to obtain 0.62 g of 7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-5-methylthiomethoxy-2,3,4,5-tetrahydro-1H-benzo[b]azepine as white amorphous solid.

1. extractionthe mixture was extracted with ethyl acetate
2. washwashed with an aqueous saturated sodium chloride solution
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationAfter filtration and concentration under reduced pressure
5. customthe residue was purified by silica gel flash chromatography (n-hexane:ethyl acetate=80:20→20:80)
6. concentrationThe purified product was concentrated under reduced pressure