反应详情

A mixture of methyl N-(2-hydroxyethyl)dithiocarbamate (3.7 g.), sodium azide (2.4 g.), water (20 ml.) and dioxane (20 ml.) was heated under reflux for four hours. After the dioxane was removed from the mixture under reduced pressure, the aqueous solution was washed with ether. The solution was adjusted to pH 1 with 10% hydrochloric acid and extracted with ethyl acetate. The extract was concentrated under reduced pressure to give oily product (0.47 g.). The oily product was purified by column chromatography on silica gel to give 1-(2-hydroxyethyl)-1H-tetrazole-5-thiol (0.17 g.). m.p. 135° to 137° C.

1. temperaturewas heated
2. temperatureunder reflux for four hours
3. customAfter the dioxane was removed from the mixture under reduced pressure
4. washthe aqueous solution was washed with ether
5. extractionextracted with ethyl acetate
6. concentrationThe extract was concentrated under reduced pressure
7. customto give oily product (0.47 g.)
8. customThe oily product was purified by column chromatography on silica gel