反应详情

温度

0 °C

Acetonitrile (460 ml) and triethylamine (87.0 ml) were added to a solution of tert-butyl {[(1R,2R,5S)-5-(dimethylcarbamoyl)-2-hydroxycyclohexyl]sulfamoyl}carbamate (138.5 g) in acetonitrile (300 ml), and the obtained solution was then cooled to approximately 0° C. Methanesulfonyl chloride (38.5 ml) was added dropwise to the reaction solution, and the obtained mixture was then stirred for approximately 30 minutes. Thereafter, water (610 ml) was added to the reaction mixture, and the obtained mixture was stirred for approximately 30 minutes. Subsequently, water (930 ml) was added to the reaction mixture, and the obtained mixture was further stirred for approximately 3 hours. Thereafter, the precipitated solid was collected by filtration and was then washed with 27.5% aqueous acetonitrile (300 ml). The obtained solid was dried under reduced pressure to obtain the title compound (138.5 g, yield: 82%).

1. stirringthe obtained mixture was stirred for approximately 30 minutes
2. stirringthe obtained mixture was further stirred for approximately 3 hours
3. filtrationThereafter, the precipitated solid was collected by filtration
4. washwas then washed with 27.5% aqueous acetonitrile (300 ml)
5. customThe obtained solid was dried under reduced pressure