반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[S:10][CH:11]=[CH:12][C:13]=2[C:14]#[N:15])=[C:4]([N+:16]([O-])=O)[CH:3]=1.O.O.[Sn](Cl)Cl>C(O)C.Cl>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2[NH:8][C:9]3[S:10][CH:11]=[CH:12][C:13]=3[C:14]([NH2:15])=[N:16][C:4]=2[CH:3]=1참가 물질
5
실험 절차
Suspend 2-(4-chloro-2-nitro-phenylamino)-thiophene-3-carbonitrile (4.85 g, 17.35 mmol) in ethanol (40.0 ml). Dissolve tin(II) chloride dihydrate (11.75 g, 52.06 mmol) in 5N HCl (40.0 ml) and then add it to the suspension. Heat the reaction at reflux for 48 hours. Cool the reaction to ambient temperature and then chill it in a refrigerator for 2 hours. Collect the resulting precipitate by vacuum filtration and then dry it under vacuum to give 3.53 g (71%) of the title compound: mass spectrum (ion spray): m/z=250.0 (M+1).
후처리
- temperatureHeat
- customthe reaction
- temperatureat reflux for 48 hours
- temperatureCool
- customthe reaction to ambient temperature
- temperaturechill it in a refrigerator for 2 hours
- customCollect the resulting precipitate
- filtrationby vacuum filtration
- customdry it under vacuum
출처 및 근거
- ORD 기록
- ord-623c2cee87cf4f29af7e5b80f35fc012
- 출처 데이터셋
- uspto-grants-2008_06
- 특허 번호
- US07384934B2
연결된 노트
불러오는 중…