反应详情

To a solution of methyl 6-({4-[({5-[(cyclopropylamino)carbonyl]-2-methylphenyl}amino)carbonyl]phenoxy}methyl)nicotinate (200 mg, 0.436)in THF(10 mL) was added LiAlH4 (33 mg, 0.871 mmol). Extra THF (7 mL) was added and the mixture was stirred for 16 h at room temperature. Glauber's salt (Na2SO4.10H2O) (1.0 g, 3.11 mmol) was added and the reaction was stirred for a further 16 h. The mixture was filtered and the solid washed with methanol (40 mL). The filtrates were evaporated and the resulting crude material was purified by SCX cartridge to give the title compound as a white solid (150 mg, 80%); NMR Spectrum: (DMSOd6) 0.57 (m, 2H), 0.67 (m, 2H), 2.25 (s, 3H), 2.85 (m, 1H), 4.56 (d, 2H), 5.28 (s, 2H), 5.59 (t, 1H), 7.15 (d, 2H), 7.34 (d, 1H), 7.51 (d, 1H), 7.64 (m, 1H), 7.79 (m, 2H), 7.97 (m, 2H), 8.37 (d, 1H), 8.55 (s, 1H), 9.83 (s, 1H); Mass Spectrum: M+H+ 432.

1. stirringthe reaction was stirred for a further 16 h
2. filtrationThe mixture was filtered
3. washthe solid washed with methanol (40 mL)
4. customThe filtrates were evaporated
5. customthe resulting crude material was purified by SCX cartridge