反应详情

温度

150 °C

Combine 1-(6-chloropyridin-3-yl)ethanone (3.4 g, 22.8 mmol), hydroxylamine (50%) in water (5.77 g, 87.4 mmol) and 0.75 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 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 afford the title compound (3.52 g, 94%). MS (ES) m/z 171 [M+1]+.

1. customSeal the vessel
2. temperatureCool the mixture to 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