反应详情

2,4-Dibromo-5-(2-fluoro-4-nitrophenoxy)benzaldehyde (13.0 g, 31.0 mmol) is refluxed with methylhydrazine (4.3 g, 93 mmol) in THF (130 mL) for 2 hours. The reaction is quenched with water (150 mL) and extracted with MTBE (2×150 mL). The organic layer is washed with saturated sodium chloride aqueous solution (2×150 mL), dried with anhydrous sodium sulfate, and concentrated to obtain a solid. The crude solid is recrystallized in EtOAc/hexane to obtain 1-(2,4-dibromo-5-(2-fluoro-4-nitrophenoxy)benzylidene)-2-methylhydrazine as a yellow solid (10.6 g, 76.7% yield). MS (m/z): 447.9 (M+H).

1. customThe reaction is quenched with water (150 mL)
2. extractionextracted with MTBE (2×150 mL)
3. washThe organic layer is washed with saturated sodium chloride aqueous solution (2×150 mL)
4. dry with materialdried with anhydrous sodium sulfate
5. concentrationconcentrated
6. customto obtain a solid
7. customThe crude solid is recrystallized in EtOAc/hexane