反应详情

温度

120 °C

N-Methylpyrrolidone (2 ml) was added to 5-[8-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purin-2-yl]-4-methylpyrimidin-2-amine (200 mg, 0.50 mmol) and piperazine (430 mg, 5.0 mmol) and the resulting mixture was stirred at 120° C. for 2 hours. 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, the residue was dissolved in tetrahydrofuran (2 ml) followed by the addition of triethylamine (140 μl, 1.0 mmol) and mesyl chloride (50 μl, 0.65 mmol) 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 (135 mg, 51%) as a white solid.

1. customThe reaction mixture was partitioned with ethyl acetate and water
2. washthe organic layer was washed with saturated brine
3. dry with materialdried over magnesium sulfate
4. customThe solvent was evaporated under reduced pressure
5. dissolutionthe residue was dissolved in tetrahydrofuran (2 ml)
6. stirringthe resulting mixture was stirred for 1 hour
7. customThe reaction mixture was partitioned with ethyl acetate 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 preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid)