反应详情

Triethylamine (2.66 mL) and hydroxylamine hydrochloride (712 mg) were added to a solution of 2,3-difluoroacetophenone (1 g) in ethanol (35 mL), and the reaction solution was heated to reflux for 3 hours. The reaction solution was returned to room temperature, and the solvent was evaporated under reduced pressure. Zinc (2.29 g) was added to a solution of the resulting residue in trifluoroacetic acid (30 mL), and the reaction solution was stirred at room temperature for 2 hours. The reaction solution was made basic with a 5 N aqueous solution of sodium hydroxide, and then extracted with chloroform. The resulting organic layer was dried over magnesium sulfate, and the solvent was evaporated under reduced pressure to obtain 1.4 g of a crude purified product containing the title compound (purity: 72 wt %). The physical properties of the compound are as follows.

1. temperaturethe reaction solution was heated
2. temperatureto reflux for 3 hours
3. customwas returned to room temperature
4. customthe solvent was evaporated under reduced pressure
5. additionZinc (2.29 g) was added to a solution of the resulting residue in trifluoroacetic acid (30 mL)
6. extractionextracted with chloroform
7. dry with materialThe resulting organic layer was dried over magnesium sulfate
8. customthe solvent was evaporated under reduced pressure
9. customto obtain 1.4 g of a crude
10. custompurified product
11. additioncontaining the title compound (purity: 72 wt %)