反应详情

1-Hydroxy-6-nitro-1,2,3-benzotriazole (7.2 g) is dissolved in 1 N aqueous sodium hydroxide (40 ml). To the solution is added dropwise methanesulfonyl chloride (5.6 g) with stirring under ice-cooling and thereto are added ethyl acetate (100 ml) and water (100 ml). The mixture is stirred at room temperature for 1 hour. To the reaction mixture is added ethyl acetate (50 ml) and the insoluble materials are filtered off. The ethyl acetate layer is dried over magnesium sulfate-charcoal. After drying, the layer is concentrated so as to be about 30 ml and thereto is added n-hexane (about 30 ml) and the mixture is allowed to stand. The precipitated crystals are separated by filtration and dried to give 1-methanesulfonyloxy-6-nitro-1,2,3-benzotriazole (7.3 g; 72%), melting point: 115°-116° c. The product is dissolved in ethyl acetate and treated with charcoal and thereto is added n-hexane to give faint yellow flakes melting point: 117°-118° C.

1. temperaturecooling
2. stirringThe mixture is stirred at room temperature for 1 hour
3. filtrationthe insoluble materials are filtered off
4. dry with materialThe ethyl acetate layer is dried over magnesium sulfate-charcoal
5. customAfter drying
6. concentrationthe layer is concentrated so as
7. additionis added n-hexane (about 30 ml)
8. customThe precipitated crystals are separated by filtration
9. customdried