2-(3,5-Dimethylphenylethynyl)-4-nitrophenylamine → HCID 21254069、化合物

HRID 1292396ノート

反応式

HRID 1292396 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:9]#[C:10][C:11]2[CH:16]=[C:15]([N+:17]([O-:19])=[O:18])[CH:14]=[CH:13][C:12]=2[NH2:20])[CH:5]=[C:6]([CH3:8])[CH:7]=1>[Pd](Cl)Cl>[CH3:1][C:2]1[CH:3]=[C:4]([C:9]2[NH:20][C:12]3[C:11]([CH:10]=2)=[CH:16][C:15]([N+:17]([O-:19])=[O:18])=[CH:14][CH:13]=3)[CH:5]=[C:6]([CH3:8])[CH:7]=1

参加物

3

反応物 1

HCID 189142732-(3,5-Dimethylphenylethynyl)-4-nitrophenylamine

生成物 1

HCID 21254069HCID 21254069、化合物収率 92%

試薬・触媒・溶媒 1

HCID 24290Palladium Chloride触媒

実験手順

To a stirred solution of 2-(3,5-dimethylphenylethynyl)-4-nitrophenylamine (50 mg in 3 mL of dry, nitrogen saturated acetonitrile) was added 5 mg of palladium (II) chloride and the mixture heated to reflux on an oil bath. After 3 hours the mixture was cooled to room temperature, concentrated in vacuo and purified by flash chromatography on silica gel (hexane:methylene chloride:ethyl acetate 15:8:1) to provide the title compound (46 mg).

後処理

  1. temperaturethe mixture heated
  2. temperatureto reflux on an oil bath
  3. concentrationconcentrated in vacuo
  4. custompurified by flash chromatography on silica gel (hexane:methylene chloride:ethyl acetate 15:8:1)

出典と根拠

ORDレコード
ord-926be2d9a99e4042bb6c4df38ee244ee
出典データセット
uspto-grants-1998_05
特許番号
US05756507

反応ノート

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