反应详情

温度

0 °C

Grignard reagent (ethyl magnesium bromide, 0.48 g, 3.6 ml 1M solution in THF, 3.64 mmol) was added drop wise to a stirred solution of 5-(4-chlorophenyl)-4-((dimethylamino)methyl)-3-(4-(N-((dimethylamino)methylene)sulfamoyl)phenyl)-N-methoxy-N-methylthiophene-2-carboxamide (compound 35e, 0.4 g, 0.72 mmol) in anhydrous THF (20 ml) at 25° C. The reaction mixture was then heated at about 70 to about 75° C. for 2 hr. The progress of the reaction was monitored by TLC. After cooling the reaction mixture to 0° C., the reaction mixture was quenched by addition of a saturated solution of ammonium chloride (15 ml). The mixture so formed was then extracted with ethyl acetate (2×30 ml). The combined organic layer was dried over anhydrous Na2SO4. The solvent from the dried organic layer was evaporated under reduced pressure to obtain a crude product, which was then purified by column chromatography over silica gel (100-200 mesh) using 60% ethyl acetate in hexanes as an eluent to obtain the title compound (0.065 g, 19.28%)

1. temperatureThe reaction mixture was then heated at about 70 to about 75° C. for 2 hr
2. customthe reaction mixture was quenched by addition of a saturated solution of ammonium chloride (15 ml)
3. customThe mixture so formed
4. extractionwas then extracted with ethyl acetate (2×30 ml)
5. dry with materialThe combined organic layer was dried over anhydrous Na2SO4
6. customThe solvent from the dried organic layer was evaporated under reduced pressure
7. customto obtain a crude product, which
8. customwas then purified by column chromatography over silica gel (100-200 mesh)