反应详情

温度

100 °C

Hydroxyamine sulfate (1.56 g, 9.504 mmol) is added to a stirred solution of 5-methoxy-4,4-dimethyl-3-oxo-pentanenitrile (2.95 g, 19.008 mmol) and sodium hydroxide (1.635 g, 40.865 mmol) in water (40 mL). The reaction mixture is heated in 100° C. oil bath for 6 hours. After this time, the reaction mixture is diluted with water and extracted with ethyl acetate 3 times. The organics are combined and washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. Purification by flash chromatography on silica gel using methanol/methylene chloride provides the title compound, m/z 171 [M+H+].

1. extractionextracted with ethyl acetate 3 times
2. washwashed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification by flash chromatography on silica gel