反应详情

温度

50 °C

To a solution of 8-(2-methoxycarbonylamino-6-methylbenzyloxy)-2-methyl-3-(2-propynyl)imidazo[1,2-a]pyridine (230 mg) in 1.4-dioxane (4.6 ml) were added 36% formaldehyde (105 mg), 50% dimethylamine in water (142 mg) and cuprous chloride (12.5 mg). After the mixture was stirred at 50° C. for 5 hours, 1.4-dioxane was evaporated under reduced pressure. The resultant residue was dissolved in chloroform (20 ml) and insoluble material was filtered off. The filtrate was washed with an aqueous solution of sodium bicarbonate and water in turn, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was recrystallized from a mixture of ethyl acetate and n-hexane to give 3-(4-N,N-dimethylamino-2-butynyl(-8-(2-methoxycarbonylamino-6-methylbenzyloxy)-2-methylimidazo-[1,2-a]pyridine (175 mg).

1. custom1.4-dioxane was evaporated under reduced pressure
2. dissolutionThe resultant residue was dissolved in chloroform (20 ml)
3. filtrationinsoluble material was filtered off
4. washThe filtrate was washed with an aqueous solution of sodium bicarbonate and water in turn
5. dry with materialdried over magnesium sulfate
6. customThe solvent was evaporated under reduced pressure
7. customthe residue was recrystallized from a mixture of ethyl acetate and n-hexane