2,5-Dichloronitrobenzene → HCID 69210302、化合物

HRID 131378

反応式

HRID 131378 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 69210302HCID 69210302、化合物収率 86.1%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-248a6419fc0248d1a6533b59d9593bae
出典データセット
uspto-grants-2008_06
特許番号
US07384934B2

関連ノート

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