Carbon Disulfide → 5-Chloro-6-iodo-1H-benzo[d]imidazole-2(3H)-thione
반응식
[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]=1참가 물질
6
실험 절차
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 resulting precipitate was collected, washed with water and a small amount of EtOH, and then dried to afford the desired product as a brown powder, which was used in the next step without further purification.
후처리
- temperatureThe mixture was heated
- temperatureat reflux for 3 h
- temperaturecooled
- filtrationfiltered
- additionTo the filtrate was added water (300 mL)
- customThe resulting precipitate was collected
- washwashed with water
- dry with materiala small amount of EtOH, and then dried
출처 및 근거
- ORD 기록
- ord-5a0e54d45a22476889bb42ebe2729721
- 출처 데이터셋
- uspto-grants-2014_11
- 특허 번호
- US08895596B2
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