反应详情

温度

100 °C

A mixture of piperidin-4-yl-(5-trifluoromethyl-[1,3,4]thiadiazol-2-yl)-amine (D4) (0.040 g, 0.16 mmol), 3,4-difluorobenzyl bromide (0.024 ml, 0.19 mmol) and diisopropylethylamine (0.042 ml, 0.24 mmol) in acetonitrile (3 ml) was stirred at 100° C. for 5 min., under microwave irradiation. After cooling to room temperature, the reaction mixture was diluted with dichloromethane and extracted with a 10% solution of ammonium chloride (25 ml). The organic layer was separated, dried (Na2SO4) and the solvent evaporated in vacuo. The crude product was purified by flash column chromatography (silica gel; 0-3% ammonia in methanol (7M)/dichloromethane) to yield E5 (0.048 g, 80%) as a solid. C15H15F5N4S requires 378. Found 379 (MH+).

1. temperatureAfter cooling to room temperature
2. extractionextracted with a 10% solution of ammonium chloride (25 ml)
3. customThe organic layer was separated
4. dry with materialdried (Na2SO4)
5. customthe solvent evaporated in vacuo
6. customThe crude product was purified by flash column chromatography (silica gel; 0-3% ammonia in methanol (7M)/dichloromethane)