反应详情

To a solution of 2-amino-N-isopropyl-benzenesulfonamide (16.1 g, 75.1 mmol) in DMI (150 mL) is added sodium hydride (6.6 g, 165.3 mmol) portionwise at 0° C. After the mixture is stirred at room temperature for one hour, 2,4,5-trichloropyrimidine (20.7 g, 112.7 mmol) is added at 0° C. After further stirring at room temperature for 5 hrs, water is added and the mixture is extracted with AcOEt three times. Organic layer is washed with brine, dried over sodium sulfate and evaporated under reduced pressure. The residue is purified by silica gel column chromatography (Hexane to Hexane:AcOEt=4:1) to afford the title compound as pale brown solid (10.2 g, 38%).

1. stirringAfter further stirring at room temperature for 5 hrs
2. extractionthe mixture is extracted with AcOEt three times
3. washOrganic layer is washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated under reduced pressure
6. customThe residue is purified by silica gel column chromatography (Hexane to Hexane:AcOEt=4:1)