反应详情

温度

25 °C

To a stirred solution of 6-hydroxy-2-benzothiazolesulfonamide (3.45 g 0.015 mole) and 4-dimethylaminopyridine (200 mg) in pyridine (25 ml) was added ethylchloroformate (1.9 ml). The reaction mixture was stirred at 25° C. for 2 hours, poured into ice and excess hydrochloric acid, extracted with ethyl acetate, washed with water, dried over magnesium sulfate and chromatographed after evaporation of the solvent on silica (150 g, 70-230 mesh) eluting with ethyl acetate-hexane 1:1 (v/v) to obtain 1.3 g of ethyl(2-sulfamoyl-6-benzothiazolyl)carbonate which melts at 144°-6° C.

1. extractionextracted with ethyl acetate
2. washwashed with water
3. dry with materialdried over magnesium sulfate
4. customchromatographed
5. customafter evaporation of the solvent on silica (150 g, 70-230 mesh)
6. washeluting with ethyl acetate-hexane 1:1 (v/v)