反应详情

6.48 g (25 mmol) of methyl 3-benzyloxypicolinate (N-oxide), 6.68 g (50 mmol) of 1-pyrrolidinylcarbonyl chloride, 6.46 g (50 mmol) of N,N-diisopropylethylamine and 7.49 g (50 mmol) of sodium iodide were refluxed under heating for two hours in 120 ml of acetonitrile. The solvent was distilled off, and water was added to the residue. The mixture was extracted with ethyl acetate, washed with a saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the obtained mixture was purified by silica gel column chromatography (ethyl acetate-n-hexane) to obtain the desired product.

1. distillationThe solvent was distilled off
2. additionwater was added to the residue
3. extractionThe mixture was extracted with ethyl acetate
4. washwashed with a saturated sodium chloride aqueous solution
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off
7. customthe obtained mixture was purified by silica gel column chromatography (ethyl acetate-n-hexane)