反应详情

温度

120 °C

To a solution of 4-[4-hydroxy-1-(4-isopropoxy-3-methyl-benzoyl)-4-piperidyl]-1-(3-pyridyl)butane-1,3-dione (1 mmol) in dichloromethane (5 mL) was added PPTS (251 mg, 1.00 mmol). The mixture was heated in microwave at 120° C. for 45 min. Water was added. The aqueous layer was extracted with dichloromethane (2×). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated to dryness. The residue was purified by column chromatography (40-50% ethyl acetate-Hex) to provide 3-(4-isopropoxy-3-methyl-benzoyl)-10-(3-pyridyl)-11-oxa-3-azaspiro[5.5]undec-9-en-8-one.

1. extractionThe aqueous layer was extracted with dichloromethane (2×)
2. washThe combined organic layers were washed with brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated to dryness
6. customThe residue was purified by column chromatography (40-50% ethyl acetate-Hex)