反应详情

To 500 ml of a solution of 26.0 g of 2-acetoxymethyl-5-(4-acetoxy-2,3,5-trimethylphenoxy)-3-methyl-3H-imidazo[4,5-b]pyridine in methanol, a 1.2 ml solution (28%) of sodium methoxide in methanol was added dropwise at −18° C., followed by stirring at the same temperature for one hour. Water was added to the reaction mixture, followed by extraction with ethyl acetate. The extract was washed with saturated saline and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue was crystallized from ethanol. The crystals were collected by filtration, whereby 20.5 g of the title compound were obtained.

1. extractionfollowed by extraction with ethyl acetate
2. washThe extract was washed with saturated saline
3. dry with materialdried over anhydrous sodium sulfate
4. distillationThe solvent was distilled off under reduced pressure
5. customThe residue was crystallized from ethanol
6. filtrationThe crystals were collected by filtration