反应详情

A mixture of 2-fluoro-4-nitrobenzene (3.2 mL, 29.7 mmol) and 1-ethylpiperazine (7.6 mL, 59.4 mmol, 2 equiv) was heated to reflux for 117 h. After cooling to rt, the reaction mixture was diluted with H2O and DCM/MeOH, 9:1. The aqueous layer was separated and extracted with DCM/MeOH, 9:1. The organic phase was washed with brine, dried (Na2SO4), filtered and concentrated. Purification of the residue by silica gel column chromatography (DCM/MeOH, 1:0→95:5) afforded 6 g of the title compound as a brown oil: ESI-MS: 236.0 [M+H]+; tR=2.49 min (System 1); TLC: Rf=0.26 (DCM/MeOH, 95:5).

1. temperaturewas heated
2. temperatureto reflux for 117 h
3. customThe aqueous layer was separated
4. extractionextracted with DCM/MeOH, 9:1
5. washThe organic phase was washed with brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification of the residue by silica gel column chromatography (DCM/MeOH, 1:0→95:5)