反应详情

A mixture of 3-chloro-N-{6-methyl-3-[3-(methyloxy)phenyl]-2-[3-(4-morpholinyl)-1-propyn-1-yl]thieno[2,3-b]pyridin-4-yl}benzenesulfonamide (Example 86) (6.8 mg, 0.012 mmol) and palladium on carbon (2.55 mg, 2.394 μmol) in ethanol (2.0 mL) was stirred under an atmosphere of hydrogen at RT for 20 h. The mixture was then filtered through celite, washing with ethanol, and evaporated to dryness. The residue was purified on silica, eluting with a gradient of 0-10% MeOH in DCM to afford the title compound (1.9 mg). 1H NMR (MeOD, 400 MHz) δ ppm: 1.76 (2H, m), 2.27-2.40 (6H, m), 2.54 (3H, s), 2.69 (2H, m), 3.61 (4H, m), 3.84 (3H, s), 6.76-6.81 (2H, m), 7.04-7.10 (1H, m), 7.27 (1H, s), 7.39-7.48 (3H, m), 7.52-7.60 (2H, m).

1. filtrationThe mixture was then filtered through celite
2. washwashing with ethanol
3. customevaporated to dryness
4. customThe residue was purified on silica
5. washeluting with a gradient of 0-10% MeOH in DCM