反应详情

温度

70 °C

To a 10% sulphuric acid aqueous solution (22 ml) of 3-propionylpyridine (Lancaster, 2.70 g, 20 mmol), trimethylacetic acid (10.21 g, 0.1 mol), silver nitrate (0.68 g, 4 mmol) and ammonium persulfate in water (36 ml) were added and the mixture was stirred for 1.5 hours at 70° C. Then, the mixture was basified with 25% ammonia solution (pH=9-10) and extracted with DCM. The organic layer was washed with brine and dried over sodium sulfate. Removal of the solvent gave a residue, which was purified by column chromatography, eluting with hexane/EtOAc (5:1), to give the title compound (3.75 g, 98%) as a yellow oil.

1. extractionextracted with DCM
2. washThe organic layer was washed with brine
3. dry with materialdried over sodium sulfate
4. customRemoval of the solvent
5. customgave a residue, which
6. customwas purified by column chromatography
7. washeluting with hexane/EtOAc (5:1)