反应详情

温度

80 °C

A mixture of piperidin-4-yl-(5-trifluoromethyl-[1,3,4]thiadiazol-2-yl)-amine (D4) (0.025 g, 0.1 mmol), 3-fluoro-4-methylbenzyl bromide (0.012 ml, 0.11 mmol) and polymer supported 1,5,7-triazabicyclo[4.4.0]dec-5-ene (2.9 mmol/g) (0.102 g, 0.30 mmol) in acetonitrile (3 ml) was stirred at 80° C. for 30 min. After cooling to room temperature, the reaction mixture was filtered through an Isolute SCX-2 cartridge. The cartridge was then washed with methanol. The crude product was eluted with a 7M solution of ammonia in methanol. The solvent was evaporated in vacuo. The crude product was purified by flash column chromatography (silica gel; 5% ammonia in methanol (7M)/dichloromethane) to yield E9 (0.017 g, 45%) as a solid. C16H18F4N4S requires 374. Found 375 (MH+).

1. temperatureAfter cooling to room temperature
2. filtrationthe reaction mixture was filtered through an Isolute SCX-2 cartridge
3. washThe cartridge was then washed with methanol
4. washThe crude product was eluted with a 7M solution of ammonia in methanol
5. customThe solvent was evaporated in vacuo
6. customThe crude product was purified by flash column chromatography (silica gel; 5% ammonia in methanol (7M)/dichloromethane)