反应详情

5-(6-Fluoro-pyridin-3-yl)-4-methyl-thiophene-2-sulfonyl chloride (310 mg, 1.06 mmol) was dissolved in dioxane and cooled with an ice-bath. Under stirring was added dropwise an excess of ammonium hydroxide solution 25%. After two hours at room temp the reaction was neutralized and the dioxane was evaporated. The reaction mixture was extracted with ethyl acetate, the combined organic extracts were washed with brine, dried over magnesiumsulfat-dihydrate, filtered and evaporated. The crude product was purified on silica-gel with eluent ethyl acetate/n-heptane to give 218 mg of the title compound as a white solid. MS (ES): m/e 271.2 (M−H)

1. temperaturecooled with an ice-bath
2. customthe dioxane was evaporated
3. extractionThe reaction mixture was extracted with ethyl acetate
4. washthe combined organic extracts were washed with brine
5. dry with materialdried over magnesiumsulfat-dihydrate
6. filtrationfiltered
7. customevaporated
8. customThe crude product was purified on silica-gel with eluent ethyl acetate/n-heptane