反应详情

温度

0 °C

6.7 g of potassium tert-butoxide were added in portions, at -20° C., while stirring and under a nitrogen atmosphere, 5 to 20 ml of trifluoroethanol. After the mixture had been warmed to 0° C., 5.2 g (30 mmol) of 2-methyl-3-methoxy-4-chloropyridine N-oxide were added in portions. The mixture was heated under reflux for 3 hours, and then left to cool down to room temperature; a further 3.45 g of potassium tert-butoxide were then added and the mixture was heated under reflux for 2 hours. After it had cooled down, 40 ml of water were added to the reaction mixture, which was then extracted with dichloromethane; the extract was then dried over MgSO4 and freed from the solvent in vacuo. The resulting oily product was subjected to further reaction.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 3 hours
3. waitleft
4. temperatureto cool down to room temperature
5. temperaturethe mixture was heated
6. temperatureunder reflux for 2 hours
7. temperatureAfter it had cooled down
8. extractionwas then extracted with dichloromethane
9. dry with materialthe extract was then dried over MgSO4
10. customThe resulting oily product was subjected to further reaction