反应详情

温度

2.5 °C

3-Methoxy-5-(trifluoromethyl)aniline. (5 g) was suspended in 20% HCl (200 mL), stirred for 30 min, cooled to 0-5° C. and diazotized with NaNO2 (2.17 g) added in small portions. The mixture was stirred for 30 min at that temperature and added dropwise to boiling water (200 mL). The mixture was refluxed for 15 min, allowed to cool to room temperature and extracted with AcOEt, dried (MgSO4), filtered and evaporated. The residue was then purified by column chromatography (silica gel; eluent: hexane and AcOEt) to give 3-methoxy-5-(trifluoromethyl)phenol (3.6 g)

1. additionadded in small portions
2. stirringThe mixture was stirred for 30 min at that temperature
3. additionadded dropwise
4. temperatureThe mixture was refluxed for 15 min
5. temperatureto cool to room temperature
6. extractionextracted with AcOEt
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customevaporated
10. customThe residue was then purified by column chromatography (silica gel; eluent: hexane and AcOEt)