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Tris(1,1-dimethylethyl)phosphine → 9-(dibenzo[b,d]furan-2-yl)-9H-3,9'-bicarbazole

HRID 1514010
ノート
印刷プレビュー

反応式

HRID 1514010 の反応式
I[C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]3[CH2:10][CH2:11][CH:12]=[CH:13][C:7]=3[C:6]=2[CH:14]=1.[CH:15]1[C:27]2[N:26]([C:28]3[CH:29]=[CH:30][C:31]4[NH:32][C:33]5[C:38]([C:39]=4[CH:40]=3)=[CH:37][CH:36]=[CH:35][CH:34]=5)[C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[C:19]=2[CH:18]=[CH:17][CH:16]=1.P(C(C)(C)C)(C(C)(C)C)C(C)(C)C.[K]>CC([O-])=O.CC([O-])=O.[Pd+2].C1(C)C(C)=CC=CC=1>[CH:14]1[C:6]2[C:7]3[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=3[O:9][C:5]=2[CH:4]=[CH:3][C:2]=1[N:32]1[C:31]2[CH:30]=[CH:29][C:28]([N:26]3[C:27]4[CH:15]=[CH:16][CH:17]=[CH:18][C:19]=4[C:20]4[C:25]3=[CH:24][CH:23]=[CH:22][CH:21]=4)=[CH:40][C:39]=2[C:38]2[C:33]1=[CH:34][CH:35]=[CH:36][CH:37]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 83681Tris(1,1-dimethylethyl)phosphineHCID 5462222PotassiumHCID 132360223,9'-BicarbazoleHCID 687356088-Iodo-3,4-dihydrodibenzo[b,d]furan

生成物 1

HCID 577031669-(dibenzo[b,d]furan-2-yl)-9H-3,9'-bicarbazole収率 82.2%

試薬・触媒・溶媒 2

HCID 167845
palladium(II) acetate
触媒
HCID 7237O-Xylene溶媒

実験手順

The 100 mL round bottom flask, equipped with magnetic stirrer and refluxed condenser, was charged with 8-iodo-3,4-dihydrodibenzo[b,d]furan (332 mg, 1 mmol), 3-(9-carbazolyl)carbazole (294 mg, 1 mmol), Pd(OAc)2 (23 mg, 10 mol %), P(t-Bu)3 (1 mL of 1M solution in toluene, 1 mmol), potassium tert-buthoxide (150 mg, 1.5 eq) and 100 ml of xylene. The flask was filled with nitrogen, and the reaction mixture was heated to reflux and stirred under nitrogen atmosphere for 24 hours. Then reaction was cooled down to room temperature, filtered through silica plug and evaporated. The residue was subjected to column chromatography on silica gel, eluent hexane/ethyl acetate mixture 9:1, providing 410 mg of 9-(dibenzo[b,d]furan-2-yl)-9H-3,9′-bicarbazole as white solid. The structure was confirmed by NMR and MS spectroscopy.

後処理

  1. customThe 100 mL round bottom flask, equipped with magnetic stirrer
  2. temperaturerefluxed condenser
  3. additionThe flask was filled with nitrogen
  4. temperaturethe reaction mixture was heated
  5. temperatureto reflux
  6. customThen reaction
  7. filtrationfiltered through silica plug
  8. customevaporated

出典と根拠

ORDレコード
ord-21bb7b40c6134599bfc49bf680235ae9
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08221905B2

反応ノート

読み込み中…

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