Carbazole → 9-(2-Bromophenyl)-9H-carbazole

HRID 923701

反応式

HRID 923701 の反応式
[CH:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[Br:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1I.C(=O)([O-])[O-].[K+].[K+]>[Cu](I)I.C1(C)C(C)=CC=CC=1>[Br:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N:12]1[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[C:5]2[C:13]1=[CH:1][CH:2]=[CH:3][CH:4]=2

参加物

6

反応物 3

HCID 6854CarbazoleHCID 114151-Bromo-2-iodobenzeneHCID 11430Potassium Carbonate

生成物 1

HCID 594650129-(2-Bromophenyl)-9H-carbazole

試薬・触媒・溶媒 2

HCID 83717Copper iodide触媒HCID 7237O-Xylene溶媒

実験手順

1.672 g of carbazole, 1.6 mL of 1-bromo-2-iodobenzene, 2.7646 g of potassium carbonate, 95 mg of copper iodide and 25 mL of xylene were refluxed in a nitrogen atmosphere. The mixture was cooled to room temperature, extracted with ethyl acetate, and dried with anhydrous magnesium sulfate to remove moisture, and the solvent was removed under reduced pressure. Silica gel column separation using a hexane solvent was conducted, thus obtaining a compound from which the solvent was then removed under reduced pressure, followed by vacuum drying, yielding 9-(2-bromophenyl)-9H-carbazole as a desired white solid intermediate.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialdried with anhydrous magnesium sulfate
  3. customto remove moisture
  4. customthe solvent was removed under reduced pressure
  5. customSilica gel column separation
  6. customthus obtaining a compound from which the solvent
  7. customwas then removed under reduced pressure
  8. customdrying

出典と根拠

ORDレコード
ord-93dd3badfbed48a3b8590f7df6e018d2
出典データセット
uspto-grants-2016_03
特許番号
US09278986B2

関連ノート

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