反应详情

A solution of 4-((4-(trifluoromethyl)benzyl)oxy)pyridine 1-oxide (350 mg) in acetic anhydride (6 ml) was heated under reflux for 4 h. The reaction mixture was then cooled to room temperature and concentrated in vacuo. The residue was diluted with MeOH (10 ml) and 2 M NaOH (10 ml), and heated at reflux for 1 h. The reaction mixture was cooled to room temperature and concentrated in vacuo. The residue was diluted with water and extracted with DCM. The DCM layer was concentrated in vacuo and purified by silica gel column chromatography (MeOH/DCM) to give the title compound (110 mg) as an off-white solid.

1. temperatureunder reflux for 4 h
2. concentrationconcentrated in vacuo
3. additionThe residue was diluted with MeOH (10 ml) and 2 M NaOH (10 ml)
4. temperatureheated
5. temperatureat reflux for 1 h
6. temperatureThe reaction mixture was cooled to room temperature
7. concentrationconcentrated in vacuo
8. additionThe residue was diluted with water
9. extractionextracted with DCM
10. concentrationThe DCM layer was concentrated in vacuo
11. custompurified by silica gel column chromatography (MeOH/DCM)