反应详情

Dissolve 1-(3-(trifluoromethyl)pyridin-2-yl)ethanol (8.8 g, 0.046 moles) in anhydrous MeOH (80 mL) and add bromine (2.35 mL) dropwise at room temperature. Reflux the mixture under N2 atmosphere for 3 weeks with the addition of bromine (1.0 mL) on each day. Concentrate the reaction mixture under vacuum, dilute with water (100 mL), neutralize with NaHCO3, extract with EtOAc (3×100 mL) and dry (MgSO4). Filter the dried extract and concentrate under vacuum to afford a yellow oil. Purify the crude product by column chromatography to afford the title compound as a pale yellow oil.

1. temperatureReflux the mixture under N2 atmosphere for 3 weeks
2. concentrationConcentrate the reaction mixture under vacuum
3. additiondilute with water (100 mL)
4. extractionextract with EtOAc (3×100 mL)
5. dry with materialdry (MgSO4)
6. filtrationFilter the dried
7. extractionextract
8. concentrationconcentrate under vacuum
9. customto afford a yellow oil
10. customPurify the crude product by column chromatography