反应详情

温度

100 °C

A mixture of C-(4-chloroquinolin-8-yl)methylamine (Preparation 89) (129 mg, 0.67 mmol), K2CO3 (186 mg, 1.34 mmol) and 4-hydroxybenzamide (110 mg, 0.81 mmol) in DMF (4 mL) were heated in a microwave at 100° C. for 40 min (150 W). Solvent removed in vacuo. The mixture was partitioned between EtOAc (50 mL) and water (20 mL), and the aqueous phase was further extracted with EtOAc (2×20 mL). The combined organic phase was washed with brine (20 mL) and dried (MgSO4). Solvent was removed in vacuo and the residue purified by column chromatography (0.25% to 0.75% NH4OH(aq), 2% to 8% MeOH in DCM) to give the title compound: RT=2.15 min; m/z (ES+)=294.1 [M+H]+.

1. customSolvent removed in vacuo
2. customThe mixture was partitioned between EtOAc (50 mL) and water (20 mL)
3. extractionthe aqueous phase was further extracted with EtOAc (2×20 mL)
4. washThe combined organic phase was washed with brine (20 mL)
5. dry with materialdried (MgSO4)
6. customSolvent was removed in vacuo
7. customthe residue purified by column chromatography (0.25% to 0.75% NH4OH(aq), 2% to 8% MeOH in DCM)