反应详情

温度

45 °C

To a solution of 3-chloro-2-fluoro-6-(methyloxy)benzaldehyde (10 g, 53.0 mmol) in 1,2-dimethoxyethane (105 mL) was added potassium carbonate (8.06 g, 58.3 mmol) and O-methylhydroxylamine hydrochloride (4.43 g, 53.0 mmol) and the mixture was stirred and heated at 45° C. for 4 hrs. After cooling, the mixture was filtered and concentrated to ˜40 mL and hydrazine monohydrate (58.3 mL, 1856 mmol) was added and the reaction was refluxed under argon over the weekend. The mixture was concentrated to 10-15 mL on the rotary evaporator and then poured into water and stirred for 10 mins. The precipitated solid was collected by filtration and washed with water (3×), sucked dry and then dried in the vacuum oven at 60° C. for 1 hr to give the title compound (D28) as an off white solid (8.83 g)

1. temperatureAfter cooling
2. filtrationthe mixture was filtered
3. additionwas added
4. temperaturethe reaction was refluxed under argon over the weekend
5. concentrationThe mixture was concentrated to 10-15 mL on the rotary evaporator
6. additionpoured into water
7. stirringstirred for 10 mins
8. filtrationThe precipitated solid was collected by filtration
9. washwashed with water (3×)
10. customsucked dry
11. customdried in the vacuum oven at 60° C. for 1 hr