反应详情

温度

0 °C

To a stirred solution of 5-(4-chlorophenyl)-1,4-dimethyl-3-(4-sulfamoylphenyl)-1H-pyrrole-2-carboxylic acid (49ε, 1.00 g, 2.47 mmol) in DMF (15 ml) was added θHOBT (0.41 g, 2.72 mmol) at room temperature, which was then followed by the addition of dimethylamine hydrochloride (0.40 g, 4.94 mmol). the reaction mixture was cooled to 0° C. and to the cooled reaction mixture was then added EDC (0.71 g, 3.70 mmol) and triethylamine (1.00 g, 1.37 ml, 9.88 mmol). The reaction mixture was then stirred at room temperature for 16 hours. The progress of the reaction was monitored by TLC. The reaction mixture was then concentrated under reduced pressure. Ethyl acetate (100 ml) was added to the residue so obtained. The mixture so obtained was then washed with saturated sodium bicarbonate solution (20 ml) followed by washing with brine (20 ml). The organic layer obtained was dried over anhydrous sodium sulphate. The dried organic layer was then concentrated under reduced pressure to obtain a crude product. The crude product was purified by column chromatography over silica gel (100-200 mesh) using 90% ethyl acetate in hexanes as an eluent to obtain the title compound (0.94 g, 88.1%).

1. concentrationThe reaction mixture was then concentrated under reduced pressure
2. additionEthyl acetate (100 ml) was added to the residue
3. customso obtained
4. customThe mixture so obtained
5. washwas then washed with saturated sodium bicarbonate solution (20 ml)
6. washby washing with brine (20 ml)
7. customThe organic layer obtained
8. dry with materialwas dried over anhydrous sodium sulphate
9. concentrationThe dried organic layer was then concentrated under reduced pressure
10. customto obtain a crude product
11. customThe crude product was purified by column chromatography over silica gel (100-200 mesh)