反应详情

Add sodium hydride (1.15 g, 28.75 mmol 60% in mineral oil) to a suspension of 2,6-dichloroisonicotinic acid (2 g, 10.42 mmol) at 0° C. in DMF (40 mL). Warm to room temperature and stir for 10 min. Add benzyl alcohol (1.35 mL, 13.045 mmol) dropwise and heat to 80° C. for 1 h. Cool to room temperature, add diiodomethane (2 mL) and stir for 30 min. Pour into saturated aqueous sodium chloride and partition between ethyl acetate and water. Dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 5:95 ethyl acetate:hexanes) to give the title compound as a colorless oil (2.3 g, 79%).

1. temperatureCool to room temperature
2. stirringstir for 30 min
3. custompartition between ethyl acetate and water
4. dry with materialDry (magnesium sulfate)
5. concentrationconcentrate
6. custompurify
7. wash(silica gel chromatography, eluting with 5:95 ethyl acetate:hexanes)