反应详情

To a well stirred solution of 1-(3,4-difluorophenyl)-2-hydroxy-propan-1-one (5.5 g, 29.6 mmol) in MeOH (200 mL) was added hydroxylamine hydrochloride (2.6 g, 38.4 mmol) and sodium acetate (8.1 g, 59.2 mmol) and the the turbid solution was stirred overnight at room temperature. The solvent was evaporated and the residue was extracted with CH2Cl2. The organic layer was washed with sat. NaHCO3, separated, dried over Na2SO4 and then filtered. The solvent was removed in vacuo to obtain 1-(3,4-difluorophenyl)-2-hydroxy-propan-1-one-oxime as an orangish yellow oil (5.8 g, 97%). It was used in the next step without purification.

1. customThe solvent was evaporated
2. extractionthe residue was extracted with CH2Cl2
3. washThe organic layer was washed with sat. NaHCO3
4. customseparated
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customThe solvent was removed in vacuo