反应详情

To the compound (2,4-difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone (22 g) in 95% ethanol (350 ml) and water (100 ml) was added NH2OH.HCl (10.1 g) and ammonium acetate (12.7 g, 2.1 eq). The resulting mixture was refluxed for 3.5 hours. The mixture was then allowed to stir at room temperature for 24 hours. The reaction mixture was concentrated to remove ethanol, poured into water (500 ml), and extracted with dichloromethane (500 ml). This was followed by washing with water, brine, and drying over magnesium sulfate. The product was concentrated to an oil and purified by column chromatography to yield 12 g of (2,4-difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone oxime.

1. temperatureThe resulting mixture was refluxed for 3.5 hours
2. concentrationThe reaction mixture was concentrated
3. customto remove ethanol
4. additionpoured into water (500 ml)
5. extractionextracted with dichloromethane (500 ml)
6. washby washing with water, brine
7. dry with materialdrying over magnesium sulfate
8. concentrationThe product was concentrated to an oil
9. custompurified by column chromatography