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Aniline → N-phenyl-3-(quinolin-2-yl)aniline

HRID 539475
ノート
印刷プレビュー

反応式

HRID 539475 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:9]1[CH:10]=[C:11]([C:15]2[CH:24]=[CH:23][C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[N:16]=2)[CH:12]=[CH:13][CH:14]=1.CC(C)([O-])C.[Na+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(C)C=CC=CC=1>[C:2]1([NH:1][C:13]2[CH:14]=[CH:9][CH:10]=[C:11]([C:15]3[CH:24]=[CH:23][C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[N:16]=3)[CH:12]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6115AnilineHCID 156059482-(3-Chlorophenyl)quinolineHCID 23676156Sodium t-butoxide

生成物 1

HCID 70654371N-phenyl-3-(quinolin-2-yl)aniline収率 46.2%

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒
HCID 1140
Toluene
溶媒

実験手順

Aniline (2.75 g, 29.6 mmol), 2-(3-chlorophenyl)quinoline (5.25 g, 21.90 mmol), sodium tert-butoxide (3.36 g, 35.0 mmol), Pd2dba3 (0.501 g, 0.548 mmol) and 2-dicyclohexylphosphino-2′,6′-dimethoxybephenyl (S-Phos) (0.898 g, 2.190 mmol) were charged into the reaction flask with 200 mL of toluene. This mixture was evacuated and back-filled with nitrogen then was heated at reflux for 20 h. The reaction mixture was cooled to room temperature then was diluted with 200 mL of water. The toluene layer was separated and the aqueous was extracted with 100 mL of toluene. The organic extracts were combined and removed under vacuum. The crude residue was passed through a silica gel column using 75% DCM/hexanes then was passed through a silica gel column using 1-5% ethyl acetate/DCM. The clean product fractions were combined and solvents were removed under vacuum yielding N-phenyl-3-(quinolin-2-yl)aniline (3 g, 10.12 mmol, 46.2% yield).

後処理

  1. customThis mixture was evacuated
  2. additionback-filled with nitrogen
  3. temperaturethen was heated
  4. temperatureat reflux for 20 h
  5. additionthen was diluted with 200 mL of water
  6. customThe toluene layer was separated
  7. extractionthe aqueous was extracted with 100 mL of toluene
  8. customremoved under vacuum
  9. customsolvents were removed under vacuum

出典と根拠

ORDレコード
ord-05307e51ba364c18b088796e4bc09239
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871361B2

反応ノート

読み込み中…

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