反应详情

温度

90 °C

A 1000 mL round bottom flask was charged with 20.0 g (123 mmol) of 4-fluorophenylhydrazine and 28.4 g (140 mmol) of 5-bromo-2-fluorobenzaldehyde and 400 mL of EtOH and warmed at 90° C. After 2 hours, the mixture was cooled to room temperature and then diluted with 200 mL of water and filtered. The solid were then dissolved in EtOAc and washed with brine. The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo. The residue was passed through a pad of silica gel to afford 37 g (97%) of N-[1-(5-bromo-2-fluorophenyl)meth-(E)-ylidene]-N′-(4-fluorophenyl)hydrazine. MS m/z 312.11 (MH+).

1. temperaturethe mixture was cooled to room temperature
2. filtrationfiltered
3. dissolutionThe solid were then dissolved in EtOAc
4. washwashed with brine
5. dry with materialThe organic layer was dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo