反应详情

A dimethyl sulfoxide solution (1.0 ml) of 5-[8-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purin-2-yl]pyrimidin-2-amine (101.9 mg, 0.26 mmol) and N-mesylpiperazine (125.8 mg, 0.77 mmol) was heated at 140° C. and stirred for 4 hours followed by the addition of N-mesylpiperazine (83.8 mg, 0.51 mmol) and the resulting mixture was further stirred at 140° C. for 3 hours. The reaction 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 reaction mixture was filtrated, then the filtrate was concentrated under reduced pressure, and the resulting residue was purified by preparative thin layer silica gel chromatography (dichloromethane:methanol=15:1) to give the title compound (89.2 mg, 68%) as a white solid.

1. stirringthe resulting mixture was further stirred at 140° C. for 3 hours
2. waitThe reaction mixture was left
3. temperatureto cool
4. washwashed with saturated aqueous sodium hydrogen carbonate solution
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. filtrationthe reaction mixture was filtrated
7. concentrationthe filtrate was concentrated under reduced pressure
8. customthe resulting residue was purified by preparative thin layer silica gel chromatography (dichloromethane:methanol=15:1)