Carbon Disulfide → 5-Chloro-6-iodo-1H-benzo[d]imidazole-2(3H)-thione
反応式
[OH-].[K+].[C:3](=[S:5])=S.[Cl:6][C:7]1[CH:8]=[C:9]([NH2:15])[C:10]([NH2:14])=[CH:11][C:12]=1[I:13]>O.CCO>[Cl:6][C:7]1[C:12]([I:13])=[CH:11][C:10]2[NH:14][C:3](=[S:5])[NH:15][C:9]=2[CH:8]=1参加物
6
実験手順
KOH (15.7 g, 238 mmol) in water (50 mL), followed by carbon disulfide (14.4 mL, 238 mmol), was added to a solution of 4-chloro-5-iodobenzene-1,2-diamine (50 g, 198 mmol) in EtOH (300 mL). The mixture was heated at reflux for 3 h, cooled and filtered. To the filtrate was added water (300 mL) and then AcOH (25 mL) in water (50 mL). The precipitate was collected, washed with water and a small amount of EtOH and dried to afford the desired product as a brown powder, which was used in the next step without further purification.
後処理
- temperatureThe mixture was heated
- temperatureat reflux for 3 h
- temperaturecooled
- filtrationfiltered
- additionTo the filtrate was added water (300 mL)
- customThe precipitate was collected
- washwashed with water
- dry with materiala small amount of EtOH and dried
出典と根拠
- ORDレコード
- ord-11312f24387c45d392369332a7e2839f
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08563746B2
反応ノート
読み込み中…