反应详情

A mixture of 3,6-difluoro-2-methyloxybenzonitrile (for a preparation see Intermediate 55) (30 g, 184 mmol) in ethanol (300 mL) was reacted with Hydrazine Monohydrate (Alfa, 89 mL, 1.84 mol, 10 equiv.). The resulting mixture was heated at reflux overnight then allowed to cool to room temperature. Silica was added to the mixture which was then evaporated to dryness. The pre-absorbed crude reaction mixture was then purified by chromatography eluting with petrol up to EtOAc (10% steps, 500 mL per step) to give the title compound (8.4 g, 25%) as a yellow solid.

1. temperatureThe resulting mixture was heated
2. temperatureat reflux overnight
3. additionSilica was added to the mixture which
4. customwas then evaporated to dryness
5. customThe pre-absorbed crude
6. customreaction mixture
7. customwas then purified by chromatography
8. washeluting with petrol up to EtOAc (10% steps, 500 mL per step)