反应详情

温度

110 °C

A mixture of tert-butyl 4-{3-[1-aminoethyl]-5-chloro-2-methoxy-6-methylphenyl}piperidine-1-carboxylate (150 mg, 0.392 mmol), 6-chloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purine (122 mg, 0.509 mmol), and sodium bicarbonate (35 mg, 0.41 mmol) in 1-butanol (4.7 mL) was degassed with N2 for ˜5 minutes. The mixture was heated at 110° C. for 3 h under nitrogen. The solvent was removed under reduced pressure and the resulting residue was diluted with EtOAc, washed with sat. NaHCO3, water, brine, dried over Na2SO4, filtered and concentrated. The residue was purified by chromatography eluting with 0 to 80% EtOAc in CH2Cl2 to provide the desired product (0.25 g). LCMS calculated for C30H42ClN6O4 (M+H)+: m/z=585.3. found: =585.3.

1. customwas degassed with N2 for ˜5 minutes
2. customThe solvent was removed under reduced pressure
3. additionthe resulting residue was diluted with EtOAc
4. washwashed with sat. NaHCO3, water, brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by chromatography
9. washeluting with 0 to 80% EtOAc in CH2Cl2