Thiosemicarbazide → 3-Formylbenzamidine-thiosemicarbazone hydrochloride
反応式
[ClH:1].[CH:2]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([NH2:9])=[NH:8])=O.[NH2:13][NH:14][C:15]([NH2:17])=[S:16]>CO.O.Cl>[ClH:1].[CH:2](=[N:13][NH:14][C:15]([NH2:17])=[S:16])[C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([NH2:9])=[NH:8]参加物
6
実験手順
A solution of 1.84 g (~0.01 mol) of crude 3-formylbenzamidine hydrochloride (prepared analogously to Example 1b) in 10 ml of methanol is added dropwise to a solution of 0.91 g (0.01 mol) of thiosemicarbazide in 5 ml of water and 10 ml of 2N hydrochloric acid. This mixture is heated under reflux for 1 hour, cooled, filtered and concentrated to dryness by evaporation. The residue is recrystallised from methanol; m.p. 210° (with decomposition). The product contains 0.5 mol of water.
後処理
- temperatureThis mixture is heated
- temperatureunder reflux for 1 hour
- temperaturecooled
- filtrationfiltered
- concentrationconcentrated to dryness by evaporation
- customThe residue is recrystallised from methanol
出典と根拠
- ORDレコード
- ord-ac0f1a49df414ef0a0926f9836542eb9
- 出典データセット
- uspto-grants-1993_08
- 特許番号
- US05238941
反応ノート
読み込み中…