反应详情

To a solution of 4.76 g (50 mmol) of 4-hydroxypyridine and 10.76 g (55 mmol) of N-chloromethylphthalimide. in 80 ml of DMF, 8.23 ml (55 mmol) of 1,8-diazabicyclo[5,4,0]-2-undecene was added. The mixture was stirred at room temperature for. 2 hours. After the solvent was distilled off, the reaction mixture was poured into water and extracted with ethyl acetate. The precipitate was filtered off. The aqueous layer was further extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain 2.67 g of the desired compound (yield: 21%, colorless crystals). mp: 129.0°-131.0° C.

1. custom2 hours
2. distillationAfter the solvent was distilled off
3. additionthe reaction mixture was poured into water
4. extractionextracted with ethyl acetate
5. filtrationThe precipitate was filtered off
6. extractionThe aqueous layer was further extracted with ethyl acetate
7. washThe organic layer was washed with water
8. dry with materialdried over anhydrous magnesium sulfate
9. distillationthe solvent was distilled off under reduced pressure
10. customThe residue was purified by column chromatography (eluent: ethyl acetate)