2,5-Dichloronitrobenzene → HCID 69210302, 화합물

HRID 131378

반응식

HRID 131378 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10].[NH2:12][C:13]1[S:14][CH:15]=[CH:16][C:17]=1[C:18]#[N:19].O.[OH-].[Li+]>CS(C)=O>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]([NH:12][C:13]2[S:14][CH:15]=[CH:16][C:17]=2[C:18]#[N:19])=[C:3]([N+:9]([O-:11])=[O:10])[CH:4]=1

참가 물질

5

반응물 3

HCID 69772,5-DichloronitrobenzeneHCID 168937Lithium hydroxide, monohydrateHCID 7366072-Aminothiophene-3-carbonitrile

생성물 1

HCID 69210302HCID 69210302, 화합물수율 86.1%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

Combine 1,4-dichloro-2-nitro-benzene (3.87 g, 20.13 mmol), 2-aminothiophene-3-carbonitrile (2.50 g, 20.13 mmol), and DMSO (25.0 ml). Add lithium hydroxide monohydrate (1.69 g, 40.27 mmol) all at once and then stir the mixture at ambient temperature for 24 hours. Pour the mixture onto ice chips and stir it for 1.5 hours. Remove the resulting orange precipitate by vacuum filtration and then dry it under vacuum to give 4.85 g (86%) of the title compound: mass spectrum (ion spray): m/z=279.1 (M+1).

후처리

  1. additionPour the mixture onto ice chips
  2. customRemove the resulting orange precipitate
  3. filtrationby vacuum filtration
  4. customdry it under vacuum

출처 및 근거

ORD 기록
ord-248a6419fc0248d1a6533b59d9593bae
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07384934B2

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