反应详情

A dimethyl sulfoxide solution (0.8 ml) of 5-[8-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purin-2-yl]pyrimidin-2-amine (76.5 mg, 0.19 mmol) and cis-2,6-dimethylpiperazine (87.5 mg, 0.77 mmol) was heated at 140° C. and stirred for 2.5 hours. The resulting mixture was left standing to cool followed by the addition of dichloromethane-methanol (10:1) and washed with saturated aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous sodium sulfate, the resulting mixture was filtrated, the filtrate was concentrated under reduced pressure, and the resulting residue was purified by preparative thin layer silica gel chromatography (dichloromethane:methanol=10:1) to give the title compound (91.1 mg, 100%) as a light brown solid.

1. waitThe resulting mixture was left
2. temperatureto cool
3. washwashed with saturated aqueous sodium hydrogen carbonate solution
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. filtrationthe resulting mixture was filtrated
6. concentrationthe filtrate was concentrated under reduced pressure
7. customthe resulting residue was purified by preparative thin layer silica gel chromatography (dichloromethane:methanol=10:1)