反应详情

To a suspension of NaH (0.73 g, 18.1 mmol, 60% in mineral oil) in DMF (10 ml) under N2 atmosphere at 0° C. was added [5-(2-Fluoro-phenyl)-3-methyl-3H-[1,2,3]triazol-4-yl]-methanol (2.5 g, 12.06 mmol) and stirred for 1 h. Then 2-chloro-5-iodopyridine (3.17 g, 13.27 mmol) was added and reaction mixture was slowly warmed to room temperature and stirred for 4 h. The reaction was monitored by TLC. The reaction mixture was quenched with ice-water, extracted with ethylacetate (50 ml), washed with brine (10 ml), dried over Na2SO4 and concentrated under reduced pressure to afford crude mass (4.4 g, 88.9% mass balance). It was triturated with hexane and the solid was filtered and dried under vacuum to furnish 2-[5-(2-Fluoro-phenyl)-3-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-5-iodo-pyridine (2.4 g, 48.48%) as yellow solid.

1. customreaction mixture
2. stirringstirred for 4 h
3. customThe reaction mixture was quenched with ice-water
4. extractionextracted with ethylacetate (50 ml)
5. washwashed with brine (10 ml)
6. dry with materialdried over Na2SO4
7. concentrationconcentrated under reduced pressure
8. customto afford crude mass (4.4 g, 88.9% mass balance)
9. customIt was triturated with hexane
10. filtrationthe solid was filtered
11. customdried under vacuum