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Bromobenzene → 9,9''-Diphenyl-9H,9'H,9''H-3,3':6',3''-tercarbazole

HRID 1050709
ノート
印刷プレビュー

反応式

HRID 1050709 の反応式
[C:1]1([N:7]2[C:19]3[CH:18]=[CH:17][C:16](B4OC(C)(C)C(C)(C)O4)=[CH:15][C:14]=3[C:13]3[C:8]2=[CH:9][CH:10]=[CH:11][CH:12]=3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[C:30]1[CH:31]=[CH:32][C:33]2[NH:34][C:35]3[C:40]([C:41]=2[CH:42]=1)=[CH:39][C:38](Br)=[CH:37][CH:36]=3.C([O-])([O-])=O.[K+].[K+].Br[C:51]1[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=1>C1(C)C=CC=CC=1.O.CCO.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:51]1([N:34]2[C:35]3[CH:36]=[CH:37][C:38]([C:11]4[CH:10]=[CH:9][C:8]5[NH:7][C:19]6[C:14]([C:13]=5[CH:12]=4)=[CH:15][C:16]([C:4]4[CH:3]=[CH:2][C:1]5[N:7]([C:19]7[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=7)[C:8]7[C:13]([C:6]=5[CH:5]=4)=[CH:12][CH:11]=[CH:10][CH:9]=7)=[CH:17][CH:18]=6)=[CH:39][C:40]=3[C:41]3[C:33]2=[CH:32][CH:31]=[CH:30][CH:42]=3)[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 7961BromobenzeneHCID 11430Potassium CarbonateHCID 2748743,6-DibromocarbazoleHCID 574156959-Phenyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)carbazole

生成物 1

HCID 593067259,9''-Diphenyl-9H,9'H,9''H-3,3':6',3''-tercarbazole収率 65.4%

試薬・触媒・溶媒 4

HCID 178418397
HCID 178418397、化合物
触媒
HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

実験手順

A solution of 9-phenyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)carbazole (7.1 g, 19.2 mmol), 3,6-dibromo-9H-carbazole (2.6 g, 8.0 mmol), K2CO3 (11.0 g, 79.7 mmol) in toluene (120 mL), water (40 mL) and EtOH (40 mL) was bubbled for 30 minutes with nitrogen. Then, Pd(PPh3)4 (0.9 g, 0.8 mmol) was added. The mixture was bubbled with nitrogen for 15 minutes and refluxed for 10 hours, after which bromobenzene (0.9 mL, 8.6 mmol) was added. The resultant mixture was refluxed for 6 hours. After cooling, the reaction mixture was extracted with CH2Cl2 and dried with MgSO4. The solvent was removed in vacuo and the residue was purified by flash chromatography using 40-60% CH2Cl2/hexane to afford 3,6-bis(9-phenylcarbazol-3-yl)carbazole (3.4 g, 65% yield) as a white solid.

後処理

  1. customThe mixture was bubbled with nitrogen for 15 minutes
  2. temperaturerefluxed for 10 hours
  3. temperatureAfter cooling
  4. extractionthe reaction mixture was extracted with CH2Cl2
  5. dry with materialdried with MgSO4
  6. customThe solvent was removed in vacuo
  7. customthe residue was purified by flash chromatography

出典と根拠

ORDレコード
ord-7f3a8502306949178ead9adfc0d8248e
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09386657B2

反応ノート

読み込み中…

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