反应详情

A mixture of 1-fluoro-3-nitrobenzene (3.2 mL, 29.7 mmol) and N-ethyl-piperazine (7.6 mL, 59.4 mmol, 2 equiv) is heated to reflux and stirred for 117 h. The reaction mixture is allowed to cool to RT and diluted with H2O (40 mL) and DCM/MeOH (9:1, 80 mL). The aqueous layer is separated and extracted with DCM/MeOH (9:1). The organic phase is washed with brine, dried (Na2SO4), filtered and concentrated. Purification of the crude product by silica gel column chromatography (DCM/MeOH, 1:0→95:5) affords the title compound as a brown oil: ESI-MS: 236.0 [MH]+; tR=2.49 min (purity: 99%, system 1); TLC: Rf=0.26 (DCM/MeOH, 95:5).

1. temperatureis heated
2. temperatureto reflux
3. customThe aqueous layer is separated
4. extractionextracted with DCM/MeOH (9:1)
5. washThe organic phase is washed with brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification of the crude product by silica gel column chromatography (DCM/MeOH, 1:0→95:5)