反应详情

温度

60 °C

A mixture of 6-piperazin-1-yl-pyridazine-3-carboxylic acid (3-methylbutyl)amide (0.255 mmol), 2-trifluoromethylbenzyl chloride (0.255 mmol), and 1,8-diazabicylco[5.4.0]undec-7-ene (0.77 mmol) was stirred and heated at 60° C. overnight. The reaction mixture was ten diluted with EtOAc (100 mL) and washed with aqueous saturated NaHCO3 (2×20 mL) and brine (2×20 mL). The organic layer was dried over anhydrous Na2SO4, concentrated, and purified by flash chromatography to give the title compound as a white solid (80 mg, 72% yield). 1H NMR (500 MHz, CDCl3) δ 8.00, 7.86, 7.82, 7.65, 7.55, 7.37, 6.95, 3.74-3.79, 3.73, 3.46-3.52, 2.62, 1.65-1.76, 1.52, 0.94. MS (ES+) m/z 436 (M+1).

1. washwashed with aqueous saturated NaHCO3 (2×20 mL) and brine (2×20 mL)
2. dry with materialThe organic layer was dried over anhydrous Na2SO4
3. concentrationconcentrated
4. custompurified by flash chromatography