反应详情

5,7-Dimethyl-2-(1,4-diazacyclooctanyl)benzoxazole (135 mg) was dissolved in methanol (3 ml), and the solution was mixed with 37% formaldehyde solution (1 ml) and 1 N hydrochloric acid (0.5 ml). This was further mixed with 10% palladium-carbon (10 mg) and stirred overnight in an atmosphere of hydrogen. After removing the catalyst by celite filtration, the filtrate was washed with ethyl acetate and then the solvent was evaporated. The thus obtained residue was extracted with 1 N hydrochloric acid and ethyl acetate, and the resulting water layer was adjusted to pH 8 with potassium carbonate and extracted with methylene chloride. The organic layer was dried with magnesium sulfate and the solvent was evaporated to obtain the title compound 5,7-dimethyl-2-(4-methyl-1,4-diazacyclooctanyl)benzoxazole (50 mg).

1. customAfter removing the catalyst
2. filtrationby celite filtration
3. washthe filtrate was washed with ethyl acetate
4. customthe solvent was evaporated
5. extractionThe thus obtained residue was extracted with 1 N hydrochloric acid and ethyl acetate
6. extractionextracted with methylene chloride
7. dry with materialThe organic layer was dried with magnesium sulfate
8. customthe solvent was evaporated