反应详情

To benzene (14 ml) are added 1-hydroxy-4-chloro-1,2,3-benzotriazole (3.4 g) and further triethylamine (2.8 ml). To the solution is added methanesulfonyl chloride (2.3 g) with stirring under ice-cooling and the mixture is stirred at the same temperature for 20 minutes and further at room temperature for 1.5 hours. After allowing to stand overnight, to the reaction mixture are added water (20 ml) and ethyl acetate (30 ml) and the ethyl acetate layer is separated. The water layer is again extracted with ethyl acetate (20 ml). The ethyl acetate extracts are combined, washed with a small amount of a saturated aqueous sodium hydrogen carbonate and water in order, dried over anhydrous sodium sulfate and the solvent is distilled off under a reduced pressure. The residue is washed with petroleum ether (10 ml) to give faint yellow crystals of 1-methanesulfonyloxy-4-chloro-1,2,3-benzotriazole (3.89 g; 79%), melting point: 71°-74° C.

1. temperaturecooling
2. stirringthe mixture is stirred at the same temperature for 20 minutes and further at room temperature for 1.5 hours
3. customthe ethyl acetate layer is separated
4. extractionThe water layer is again extracted with ethyl acetate (20 ml)
5. washwashed with a small amount of a saturated aqueous sodium hydrogen carbonate and water in order
6. dry with materialdried over anhydrous sodium sulfate
7. distillationthe solvent is distilled off under a reduced pressure
8. washThe residue is washed with petroleum ether (10 ml)