Water → HCID 178444732、化合物
反応式
[N-:1]=[N+:2]=[N-:3].[Na+].O.[CH2:6]([NH:12][C:13](=[S:16])SC)[CH2:7][CH2:8][CH2:9][CH2:10][CH3:11]>C(O)C>[CH2:6]([N:12]1[C:13]([SH:16])=[N:3][N:2]=[N:1]1)[CH2:7][CH2:8][CH2:9][CH2:10][CH3:11]参加物
5
反応条件
- 温度
- 90 °C
実験手順
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.).
後処理
- distillationEthanol was distilled off from the reaction mixture
- washthe residue was washed with diethyl ether (1 l.)
- extractionextracted with diethyl ether (1 l.)
- washThe extract was washed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-27ca43c30aed4462a2db0e46c8cf720d
- 出典データセット
- uspto-grants-1985_01
- 特許番号
- US04493833
反応ノート
読み込み中…