反应详情

温度

95 °C

Add 5-hydroxy-2-methyl-pyridine (3.3 g, 30.6 mmol), potassium carbonate (17 g, 122.4 mmol) and 2-bromo-1,1,1-trifluoroethane (10 g, 61.2 mmol) to a flask containing DMF (60 mL) and heat to 95° C. for 20 h. Cool the mixture, dilute with aqueous 10% NaCl (20 mL) and extract with hexane/EtOAc (1:1, 100 mL). Filter the bi-phasic mixture through Celite®, separate and wash the organic layer with aqueous 10% NaCl (3×50 mL) and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (9:1 to 1:1) to obtain the desired intermediate (4.1 g, 70%).

1. temperatureCool the mixture
2. extractionextract with hexane/EtOAc (1:1, 100 mL)
3. filtrationFilter the bi-phasic mixture through Celite®
4. customseparate
5. washwash the organic layer with aqueous 10% NaCl (3×50 mL)
6. concentrationconcentrate in vacuo
7. customPurify by chromatography on silica gel eluting with hexane/EtOAc (9:1 to 1:1)