反应详情

温度

90 °C

Sodium azide (155.9 g.) and water (0.8 l.) were added under stirring to a solution of methyl N-hexyldithiocarbamate (430 g.) in ethanol (1.7 l.) and the resulting mixture was refluxed for 3.5 hours at 90° C. Ethanol was distilled off from the reaction mixture and the residue was washed with diethyl ether (1 l.), adjusted to pH 2.0 with conc. hydrochloric acid and extracted with diethyl ether (1 l.). The extract was washed with water, dried over magnesium sulfate and concentrated to give an oil of 1-hexyl-1H-tetrazole-5-thiol (431.3 g.).

1. distillationEthanol was distilled off from the reaction mixture
2. washthe residue was washed with diethyl ether (1 l.)
3. extractionextracted with diethyl ether (1 l.)
4. washThe extract was washed with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated