反应详情

温度

65 °C

20 g (0.134 mol) of 3-pyridyl isopropyl ketone and 30.2 g (0.268 mol) of potassium tert-butylate were dissolved in 200 ml of tert-butanol. Thereafter, 37.4 g (0.208 mol) of trimethylsulfonium iodide were added and the mixture was heated at 65° C. for 1.5 hours. The inorganic salts were separated off and the reaction solution was evaporated down, after which 75 ml of half-concentrated H2SO4 were added to the crude product and the mixture was heated at 60°-70° C. for 8 hours. The pH was then brought to 9 with 4N NaOH solution and extraction was carried out with methylene chloride. The organic phase was dried and evaporated down and the product was then purified by chromatography.

1. customThe inorganic salts were separated off
2. customthe reaction solution was evaporated down
3. additionafter which 75 ml of half-concentrated H2SO4 were added to the crude product
4. temperaturethe mixture was heated at 60°-70° C. for 8 hours
5. extractionThe pH was then brought to 9 with 4N NaOH solution and extraction
6. customThe organic phase was dried
7. customevaporated down
8. customthe product was then purified by chromatography