反应详情

With cooling with ice, oxalyl chloride (5.8 mL) and DMF (3 drops) were added to a CHCl3 (40 mL) solution of 2-chloro-6-benzyloxypyridine-4-carboxylic acid, and stirred at that temperature for 1 hour. DMF (3 drops) was added to it, and stirred overnight at room temperature, then oxalyl chloride (2.9 mL) and DMF (3 drops) were added to it, and stirred at room temperature for 3 hours. The solvent was evaporated away, CHCl3-MeOH was added to the residue, and stirred at room temperature for 30 minutes. Sodium bicarbonate water was added to the reaction solution, extracted with chloroform, and the organic layer was washed with water, saturated sodium bicarbonate water and saturated saline water, and dried with anhydrous sodium sulfate. This was filtered, concentrated under reduced pressure, and the residue was purified through silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound as a yellow oil.

1. stirringstirred overnight at room temperature
2. stirringstirred at room temperature for 3 hours
3. customThe solvent was evaporated away
4. additionCHCl3-MeOH was added to the residue
5. stirringstirred at room temperature for 30 minutes
6. additionSodium bicarbonate water was added to the reaction solution
7. extractionextracted with chloroform
8. washthe organic layer was washed with water, saturated sodium bicarbonate water and saturated saline water
9. dry with materialdried with anhydrous sodium sulfate
10. filtrationThis was filtered
11. concentrationconcentrated under reduced pressure
12. customthe residue was purified through silica gel column chromatography (hexane/ethyl acetate)