反应详情

温度

90 °C

To 3-chloro-4-(trifluoromethyl)phenol (Preparation 16, 110 mg, 0.56 mmol) and 5-chloro-2,4-difluoro-N-(methylsulfonyl)benzamide (Preparation 13, 150 mg, 0.56 mmol) dissolved in dimethylsulfoxide (5 ml) was added potassium carbonate (232 mg, 1.68 mmol) and the mixture stirred at 90° C. for 18 hours under nitrogen. The mixture was poured onto ammonium chloride (aq) and extracted with ethyl acetate (3×20 mL), washed with water (3×20 mL) and dried (MgSO4). Purification of the crude product by silica gel column chromatography using 80% Ethyl acetate in heptane furnished the title compound as white solid (12.2 mg, 4.9%).

1. additionThe mixture was poured onto ammonium chloride (aq)
2. extractionextracted with ethyl acetate (3×20 mL)
3. washwashed with water (3×20 mL)
4. dry with materialdried (MgSO4)
5. customPurification of the crude product by silica gel column chromatography