反应详情

To 400 ml of a solution of 38.0 g of 2-hydroxymethyl-5-(4-hydroxy-2,3,5-trimethylphenoxy)-3-methyl-3H-imidazo[4,5-b]pyridine in pyridine, 69 ml of acetic anhydride were added dropwise under ice cooling. After stirring at room temperature for 3 hours, the reaction mixture was allowed to stand overnight at room temperature. The solvent was distilled off under reduced pressure. Water was added to the residue, followed by extraction with ethyl acetate. The extract was washed with saturated saline and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue was separated and purified by chromatography through a silica gel column (eluting solvent n-hexane/ethyl acetate=1/2), whereby 39.5 g of the title compound were obtained.

1. waitto stand overnight at room temperature
2. distillationThe solvent was distilled off under reduced pressure
3. additionWater was added to the residue
4. extractionfollowed by extraction with ethyl acetate
5. washThe extract was washed with saturated saline
6. dry with materialdried over anhydrous sodium sulfate
7. distillationThe solvent was distilled off under reduced pressure
8. customThe residue was separated
9. custompurified by chromatography through a silica gel column (eluting solvent n-hexane/ethyl acetate=1/2)