反应详情

A yellow solution of 5-(2,6-dimethoxyphenyl)-5-((quinolin-3-ylmethyl)amino)pentanoic acid (1.074 g; 2.72 mmol; 1.0 equiv.) in anh. DMF (50 ml) was treated successively with HATU (1.294 g; 3.40 mmol; 1.25 equiv.) and with DIPEA (0.59 ml; 3.40 mmol; 1.25 equiv.). The resulting orange solution was stirred at rt, under nitrogen, for 2 h45. Water (100 ml) and Et2O (100 ml) were then added, and the separated aq. layer was further extracted with Et2O (3×100 ml). The mixed organic layers were washed with water (15 ml) and with brine (15 ml), dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure. Purification by FC (DCM/MeOH=20/1) afforded 6-(2,6-dimethoxyphenyl)-1-(quinolin-3-ylmethyl)piperidin-2-one as a beige solid. LC-MS (conditions B): tR=0.68 min.; [M+H]+: 377.36 g/mol.

1. extractionthe separated aq. layer was further extracted with Et2O (3×100 ml)
2. washThe mixed organic layers were washed with water (15 ml) and with brine (15 ml)
3. dry with materialdried over anh. MgSO4
4. filtrationfiltered
5. concentrationconcentrated to dryness under reduced pressure
6. customPurification by FC (DCM/MeOH=20/1)