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Dichlorodiphenylsilane → (3-Bromophenyl)diphenyl(triphenylen-2-yl)silane

HRID 241501
ノート
印刷プレビュー

反応式

HRID 241501 の反応式
C([Li:5])CCC.CCCCCC.[Br:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([Br:19])[CH:14]=1.Cl[Si:21](Cl)([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.[C:35]1([Li])[C:52]2[C:51]3[C:46](=[CH:47][CH:48]=[CH:49][CH:50]=3)[C:45]3[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=3)[C:39]=2[CH:38]=[CH:37][CH:36]=1.Cl[SiH](Cl)C1C=CC=CC=1>CCOCC>[Br:12][C:13]1[CH:14]=[C:15]([Li:5])[CH:16]=[CH:17][CH:18]=1.[Br:19][C:15]1[CH:14]=[C:13]([Si:21]([C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:36]2[CH:37]=[CH:38][C:39]3[C:40]4[C:45](=[CH:44][CH:43]=[CH:42][CH:41]=4)[C:46]4[C:51](=[CH:50][CH:49]=[CH:48][CH:47]=4)[C:52]=3[CH:35]=2)[CH:18]=[CH:17][CH:16]=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 6

HCID 6627DichlorodiphenylsilaneHCID 79271,3-DibromobenzeneHCID 8058HexaneHCID 74207Dichloro(phenyl)silaneHCID 178418339ButyllithiumHCID 178506667HCID 178506667、化合物

生成物 2

HCID 86684651
(3-Bromophenyl)diphenyl(triphenylen-2-yl)silane
収率 75%
HCID 178506674HCID 178506674、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

Into a suspension of 2-bromotriphenylene (7.28 g, 23.70 mmol) in ether (50 mL) was added n-butyllithium solution in hexane (14.81 mL, 23.70 mmol) dropwise at −78° C. The suspension was gradually warmed to 0° C. and stirred for 3 hours to yield a solution of triphenylenyllithium. In a separate flask a solution of 3-bromophenyllithium was prepared by dropwise addition of n-butyllithium solution in hexane (14.81 mL, 23.70 mmol) into a solution of 1,3-dibromobenzene (2.87 mL, 23.70 mmol) in ether (50 mL). The solution was stirred at this temperature for 2.5 hours before being transferred into a solution of dichlorodiphenylsilane (4.88 mL, 23.70 mmol) in ether (30 mL) at −78° C. After stirring for another 2 h, the triphenylenyllithium solution prepared above was introduced dropwise into the flask containing the dichlorophenylsilane. The reaction mixture was allowed to gradually warm to room temperature and was stirred overnight. The mixture was quenched with water and the organic phase was isolated. Upon evaporation of the solvent, the residue was purified by column chromatography on silica gel with hexane/DCM (85/15, v/v) as eluent to yield (3-bromophenyl)diphenyl(triphenylen-2-yl)silane (8.5 g, 75%) as a white powder.

後処理

  1. stirringAfter stirring for another 2 h
  2. additionabove was introduced dropwise into the flask
  3. stirringwas stirred overnight
  4. customThe mixture was quenched with water
  5. customthe organic phase was isolated
  6. customUpon evaporation of the solvent
  7. customthe residue was purified by column chromatography on silica gel with hexane/DCM (85/15

出典と根拠

ORDレコード
ord-eb95efb52ae145e2abfbd0c227366ae9
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08652656B2

反応ノート

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