反应详情

With cooling with ice, benzyl alcohol (3.4 mL) was dropwise added to a DMF (100 mL) suspension of sodium hydride (3.2 g). This was stirred at that temperature for 1 hour, then a DMF (30 mL) solution of 2,6-dichloropyridine-4-carboxylic acid (6.38 g) was dropwise added to the reaction solution with cooling with ice, and stirred at that temperature for 1 hour and 30 minutes and then overnight at 90° C. With cooling with ice, diluted hydrochloric acid was added to it, and extracted with ethyl acetate. The organic layer was washed with saturated saline water, dried with anhydrous sodium sulfate, filtered and concentrated under reduced pressure. A mixed solution of hexane/ethyl acetate=2/1 was added to the residue, and the formed precipitate was removed. The filtrate was concentrated under reduced pressure to obtain the title compound as a yellow oil. Not purified, this was used in the next step.

1. temperaturewith cooling with ice
2. stirringstirred at that temperature for 1 hour and 30 minutes
3. customovernight
4. customat 90° C
5. additionwas added to it
6. extractionextracted with ethyl acetate
7. washThe organic layer was washed with saturated saline water
8. dry with materialdried with anhydrous sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure
11. additionA mixed solution of hexane/ethyl acetate=2/1 was added to the residue
12. customthe formed precipitate was removed
13. concentrationThe filtrate was concentrated under reduced pressure