反应详情

温度

60 °C

To a stirred suspension of 672 mg of N-[(5S)-3-(3-fluoro-4-piperazine-1-yl-phenyl)-2-oxo-oxazolidin-5-ylmethyl]-acetamide (2 mmol) and 0.42 ml of triethylamine (3 mmol) in 30 ml dichloromethane was added at rt. a solution of 484 mg bromoacetylbromide (2.4 mmol) in 2 ml of dichloromethane. The reaction was monitored by TLC. The reaction solution was washed with water and brine, the dichloromethane layer dried over Mg sulfate, filtered and the filtrate evaporated to dryness. The residue was digested in 20 ml ether, the solid filtered and dried. The colorless solid was dissolved in 10 ml DMF, 372 mg N-Boc piperazine 2 mmol) and 276 mg of potassium carbonate (2 mmol) were added. The reaction was stirred over night at 60° C. and monitored by TLC. The DMF was evaporated to dryness, the residue purified by chromatography, using a 19/1 dichloromethane/methanol mixture as eluent.

1. additionwas added at rt
2. washThe reaction solution was washed with water and brine
3. dry with materialthe dichloromethane layer dried over Mg sulfate
4. filtrationfiltered
5. customthe filtrate evaporated to dryness
6. filtrationthe solid filtered
7. customdried
8. dissolutionThe colorless solid was dissolved in 10 ml DMF
9. customThe DMF was evaporated to dryness
10. customthe residue purified by chromatography