反应详情

A solution of N-[5-(3,5-dichloro-4-sulfamoyl-phenyl)-4-methyl-thiazol-2-yl]-acetamide (Example 6) (0.70 g, 1.84 mmol) in aqueous hydrochloric acid (5M, 10 ml) and ethanol (20 ml) is heated at reflux for 90 minutes. When cool, the mixture is concentrated to remove ethanol and the aqueous solution is brought to pH 9 by addition of aqueous sodium hydroxide (4M). The product is extracted with n-butanol (50 ml) and the organic extract is dried over MgSO4. Removal of the solvent followed by chromatography on silica (eluting with ethyl acetate—hexane, 2:1 increasing to 4:1) affords the title compd. MH+ (MS, AP+): 337.8, 339.5

1. temperatureat reflux for 90 minutes
2. temperatureWhen cool
3. concentrationthe mixture is concentrated
4. customto remove ethanol
5. additionthe aqueous solution is brought to pH 9 by addition of aqueous sodium hydroxide (4M)
6. extractionThe product is extracted with n-butanol (50 ml)
7. extractionthe organic extract
8. dry with materialis dried over MgSO4
9. customRemoval of the solvent
10. customaffords the title