反应详情

To a solution of methyl N-(2-acetamidoethyl)dithiocarbamate (12.6 g.) in dioxane (40 ml.) was added a solution of sodium azide (6.4 g.) in water (40 ml.), and the mixture was heated under reflux for 4 hours. After dioxane was removed from the resultant mixture under reduced pressure, the residue was washed with ether (350 ml.) and adjusted to pH 1 with 10% hydrochloric acid. After the resultant solution was extracted with ethyl acetate (1.5 l.), the extract was dried over magnesium sulfate and the solvent was evaporated to dryness to give 1-(2-acetamidoethyl)-1H-tetrazole-5-thiol (5.3 g.) having m.p. 137.5° to 139.5° C.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 4 hours
3. customAfter dioxane was removed from the resultant mixture under reduced pressure
4. washthe residue was washed with ether (350 ml.)
5. extractionAfter the resultant solution was extracted with ethyl acetate (1.5 l.)
6. dry with materialthe extract was dried over magnesium sulfate
7. customthe solvent was evaporated to dryness