反应详情

温度

150 °C

A solution of 2-[6-(4-chloro-benzyl)-2-(piperidin-4-ylamino)-pyrimidin-4-yl]-propan-2-ol (76 mg, 0.19 mmol), 4-chloro-2-picoline (24 mg, 0.19 mmol) and triethylamine (53 μL, 0.38 mmol) in sulfolane (0.76 mL) was stirred in a preheated oil bath at 150° C. for 30 minutes. After further addition of 4-chloro-2-picoline (24 mg, 0.19 mmol) and triethylamine (53 μL, 0.38 mmol) the solution was stirred for further 60 minutes at 150° C. It was diluted with ethyl acetate (15 mL) and was washed with 1 M aqueous sodium carbonate solution (20 mL), water (15 mL) and brine (15 mL). The combined aqueous layers were extracted with ethyl acetate (15 mL). The organic layer was dried over sodium sulfate. Concentration and purification by chromatography (SiO2, dichloromethane/methanol/triethylamine=95:4.5:0.5) afforded the title compound (34 mg, 40%) as an off-white foam.

1. washwas washed with 1 M aqueous sodium carbonate solution (20 mL), water (15 mL) and brine (15 mL)
2. extractionThe combined aqueous layers were extracted with ethyl acetate (15 mL)
3. dry with materialThe organic layer was dried over sodium sulfate
4. concentrationConcentration and purification by chromatography (SiO2, dichloromethane/methanol/triethylamine=95:4.5:0.5)