2-(3,5-Dimethylphenylethynyl)-4-nitrophenylamine → HCID 21254069, 화합물

HRID 1292396노트

반응식

HRID 1292396 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

HCID 21254069HCID 21254069, 화합물수율 92%

시약·촉매·용매 1

HCID 24290Palladium Chloride촉매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-926be2d9a99e4042bb6c4df38ee244ee
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05756507

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