反应详情

温度

50 °C

To a solution of 4-(8-aminomethylquinolin-4-yloxy)benzamide (23 mg, 0.08 mmol, Preparation 90) in MeOH (5 mL) was added 3-methylbutyraldehyde (8.5 μL, 0.08 mmol) and 4 Å molecular sieves (500 mg). The resulting mixture was heated to 50° C. for 16 h then cooled to rt and NaBH4 (6 mg, 0.16 mmol) was added. After 3 h a few drops of water were added, the mixture filtered and washed with MeOH. Solvent was removed in vacuo and the residue purified by column chromatography (0.25% NH4OH(aq), 5% MeOH in DCM) to give the title compound: RT=2.65 min; m/z (ES+)=364.2 [M+H]+.

1. temperaturethen cooled to rt
2. filtrationthe mixture filtered
3. washwashed with MeOH
4. customSolvent was removed in vacuo
5. customthe residue purified by column chromatography (0.25% NH4OH(aq), 5% MeOH in DCM)