反应详情

温度

100 °C

A mixture of commercially available 1-chloro-3,5-dimethoxybenzene (1.243 g; 6.98 mmol), P2O5(991 mg; 6.98 mmol), and methanesulfonic acid (5.659 g; 58.89 mmol) was treated with commercially available (S)-6-oxopiperidine-2-carboxylic acid (1.000 g; 6.98 mmol), and the resulting mixture was heated to 100° C. for 30 min. After cooling to rt, water was added, and the resulting solution was extracted with DCM. The mixed organic layers were dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure. Purification by preparative HPLC afforded 6-(4-chloro-2,6-dimethoxyphenyl)piperidin-2-one as a colorless solid. LC-MS (conditions E): tR=0.61 min.; [M+H]+: 270.26 g/mol.

1. temperatureAfter cooling to rt
2. extractionthe resulting solution was extracted with DCM
3. dry with materialThe mixed organic layers were dried over anh. MgSO4
4. filtrationfiltered
5. concentrationconcentrated to dryness under reduced pressure
6. customPurification by preparative HPLC