反应详情

温度

60 °C

A mixture of 1-bromo-2-fluoro-3-nitrobenzene (4.1 g, 18.6 mmol) and cyclopropanamine (1.29 mL, 18.6 mmol) in THF (10 mL) was stirred under N2 at 60° C. for 18 h. The reaction mixture was diluted with EtOAc, washed with water, filtered on a pad of Celite™, washed with brine and dried over magnesium sulfate. The solution was concentrated in vacuo. Purification of the residue by flash chromatography on a silica gel column using 30 to 50% gradient of DCM in hexane as eluent gave 2-bromo-N-cyclopropyl-6-nitroaniline: LC-MS (ESI) m/z 259.0 [M+H]+.

1. washwashed with water
2. filtrationfiltered on a pad of Celite™
3. washwashed with brine
4. dry with materialdried over magnesium sulfate
5. concentrationThe solution was concentrated in vacuo
6. customPurification of the residue by flash chromatography on a silica gel column