反应详情

温度

120 °C

N-Methylpyrrolidone (1 ml) was added to 5-[8-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purin-2-yl]-4-methylpyrimidin-2-amine (100 mg, 0.25 mmol) and 3-methylaminopyrrolidine (130 mg, 1.5 mmol) and the resulting mixture was stirred at 120° C. for 0.5 hours. The reaction mixture was partitioned with chloroform and saturated brine and the organic layer was washed with saturated brine and dried over magnesium sulfate. The solvent was concentrated under reduced pressure, triethylamine (100 μl, 0.75 mmol) and mesyl chloride (60 μl, 0.75 mmol) were added to the residue, and the resulting mixture was stirred for 1 hour. The reaction mixture was partitioned with ethyl acetate (containing a small amount of tetrahydrofuran) and water and the organic layer was washed with saturated brine and dried over magnesium sulfate. The solvent was evaporated under reduced pressure and then the residue was purified by silica gel chromatography (chloroform:methanol=9:1) to give a pale yellow solid (75 mg, 50%).

1. customThe reaction mixture was partitioned with chloroform and saturated brine
2. washthe organic layer was washed with saturated brine
3. dry with materialdried over magnesium sulfate
4. additionwere added to the residue
5. stirringthe resulting mixture was stirred for 1 hour
6. customThe reaction mixture was partitioned with ethyl acetate (
7. additioncontaining a small amount of tetrahydrofuran) and water
8. washthe organic layer was washed with saturated brine
9. dry with materialdried over magnesium sulfate
10. customThe solvent was evaporated under reduced pressure
11. customthe residue was purified by silica gel chromatography (chloroform:methanol=9:1)