反应详情

温度

100 °C

A mixture of 2-(2-(2-fluoro-5- nitrophenoxy)ethoxy)tetrahydro-2H-pyran XXII (1550 mg, 5.43 mmol), 1-(oxetan-3-yl)piperazine (772 mg, 5.43 mmol) and potassium carbonate (1126.41 mg, 8.15 mmol) in NMP (6 mL) was stirred at 100° C. for 8 h. The aqueous layer was separated and extracted with EtOAc. The combined organic extracts were washed with H2O (5× to remove NMP) and brine and dried over sodium sulfate. The resulting residue was purified by column chromatography ISCO Rf (24 g column) eluting with a gradient of 100% DCM—60:35:5 DCM:Et2O:MeOH to provide 1-(4-nitro-2-(2-((tetrahydro-2H-pyran-2-yl)oxy)ethoxy)phenyl)-4-(oxetan-3-yl)piperazine XXIII.

1. customThe aqueous layer was separated
2. extractionextracted with EtOAc
3. washThe combined organic extracts were washed with H2O (5× to remove NMP) and brine
4. dry with materialdried over sodium sulfate
5. customThe resulting residue was purified by column chromatography ISCO Rf (24 g column)
6. washeluting with a gradient of 100% DCM—60:35:5 DCM