反应详情

温度

75 °C

A sealed tube containing a mixture of methyl 5-oxo-5-(2,4,6-trimethoxyphenyl)pentanoate (200 mg; 0.67 mmol), ammonium acetate (520 mg; 6.75 mmol), and NaBH3CN (44 mg; 0.67 mmol) in anh. MeOH (3 ml) was heated to 75° C. for 18 h. After cooling to rt, 2 M aq. HCl was added, and the volatiles were removed under reduced pressure. The aq. solution was extracted with DCM (3×20 ml), and the mixed organic layers were dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure. Purification by FC (DCM/MeOH=25/1) afforded 6-(2,4,6-trimethoxyphenyl)piperidin-2-one as a colorless solid. LC-MS (conditions D): tR=0.86 min.; [M+H]+: 266.84 g/mol.

1. additionA sealed tube containing
2. temperatureAfter cooling to rt
3. customthe volatiles were removed under reduced pressure
4. extractionThe aq. solution was extracted with DCM (3×20 ml)
5. dry with materialthe mixed organic layers were dried over anh. MgSO4
6. filtrationfiltered
7. concentrationconcentrated to dryness under reduced pressure
8. customPurification by FC (DCM/MeOH=25/1)