反应详情

A procedure similar to that described in Preparation 15 was repeated, except that the reaction was conducted using 3.00 g of 6-bromo-2-hydroxymethyl-3H-imidazo-[4,5-b]pyridine (prepared as described in Preparation 58), 0.58 g of sodium hydride (as a 55% by weight dispersion in mineral oil), 0.92 ml of methyl iodide and 60 ml of dimethylformamide. After completion of the reaction with methyl iodide, the reaction mixture was freed from dimethylformamide by distillation under reduced pressure. The residue was diluted with water, after which it was extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, after which the solvent was removed by distillation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, using a 50:1 by volume mixture of ethyl acetate and methanol as the eluent, to give 1.40 g of the title compound, melting at 142°-144° C.

1. customA procedure similar to that described in Preparation 15
2. distillationthe reaction mixture was freed from dimethylformamide by distillation under reduced pressure
3. additionThe residue was diluted with water
4. extractionafter which it was extracted with ethyl acetate
5. washThe extract was washed with an aqueous solution of sodium chloride
6. dry with materialdried over anhydrous sodium sulfate
7. customafter which the solvent was removed by distillation under reduced pressure
8. customThe resulting residue was purified by column chromatography through silica gel
9. additionby volume mixture of ethyl acetate and methanol as the eluent