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 ethylenediamine (150 mg, 2.49 mmol) and the resulting mixture was stirred at 120° C. for 3.5 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, then triethylamine (100 μl, 0.75 mmol) and mesyl chloride (25 μl, 0.32 mmol) were added to the residue, and the resulting mixture was stirred for 1 hour. The reaction mixture was partitioned with ethyl acetate 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 preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid) to give the title compound (57 mg, 46%) as a pale yellow solid.

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. concentrationThe solvent was concentrated under reduced pressure
5. stirringthe resulting mixture was stirred for 1 hour
6. customThe reaction mixture was partitioned with ethyl acetate and water
7. washthe organic layer was washed with saturated brine
8. dry with materialdried over magnesium sulfate
9. customThe solvent was evaporated under reduced pressure
10. customthe residue was purified by preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid)