carbazic acid, dithio-, monopotassium salt → Ethyl 5-sulfanyl-1,3,4-thiadiazole-2-carboxylate
反応式
[CH2:1]([O:3][C:4](=[O:9])[C:5](SC)=S)[CH3:2].[NH:10]([C:12]([S-:14])=[S:13])[NH2:11].[K+]>C(O)C>[SH:13][C:12]1[S:14][C:5]([C:4]([O:3][CH2:1][CH3:2])=[O:9])=[N:11][N:10]=1参加物
4
実験手順
Ethyl(methylthio)(thioxo)acetate (20.0 g, 122 mmol) and potassium hydrazinecarbodithioate (R. S. Drago et al., JACS (1983) 105, 2287) (17.8 g, 122 mmol) were reflux overnight in ethanol (500 ml). The solution was concentrated and EtOAc was added. The organic phase was washed with 1M HCl, brine and dried over anhydrous Na2SO4. The solvent was evaporated and the residue purified on silica gel (hexanes-acetone, 80:20) to give the title compound. 1H NMR (400 MHz, acetone-d6): 4.43 (q, 2H), 1.38 (t, 3H).
後処理
- concentrationThe solution was concentrated
- additionEtOAc was added
- washThe organic phase was washed with 1M HCl, brine
- dry with materialdried over anhydrous Na2SO4
- customThe solvent was evaporated
- customthe residue purified on silica gel (hexanes-acetone, 80:20)
出典と根拠
- ORDレコード
- ord-46f267bc728043b4ad6218c483c21f94
- 出典データセット
- uspto-grants-2009_06
- 特許番号
- US07553973B2
反応ノート
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