反应详情

温度

150 °C

Combine 1-(2-bromo-phenyl)-ethanone (4.5 g, 22.6 mmol), 50% hydroxylamine in water (2.3 g, 69.6 mmol) and 1 mL of acetic acid in 15 mL of dioxane in a pressure vessel. Seal the vessel and heat the mixture in an oil bath for 3 h at 150° C. Cool the mixture to room temperature (RT). Dilute with chloroform/IPA (3/1), wash with water and aqueous saturated sodium chloride. Separate the layers and dry the organic layer over sodium sulfate. Concentrate in vacuo to give the crude product. Purify by column chromatography (20% THF in dichloromethane (DCM) to give the title compound (4.0 g, 83%). MS (ES) m/z 214/216 [M+1]+.

1. customSeal the vessel
2. temperatureCool the mixture to room temperature (RT)
3. washwash with water and aqueous saturated sodium chloride
4. customSeparate the layers
5. dry with materialdry the organic layer over sodium sulfate
6. concentrationConcentrate in vacuo
7. customto give the crude product
8. customPurify by column chromatography (20% THF in dichloromethane (DCM)