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Toluene → 2-bromo-9,9-dimethyl-7-(naphthalene-2-yl)-9H-fluorene

HRID 1429318
ノート
印刷プレビュー

反応式

HRID 1429318 の反応式
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1B(O)O.[Br:14][C:15]1[CH:27]=[CH:26][C:25]2[C:24]3[C:19](=[CH:20][C:21](I)=[CH:22][CH:23]=3)[C:18]([CH3:30])([CH3:29])[C:17]=2[CH:16]=1.C1(C)C=CC=CC=1.C(=O)([O-])[O-].[Na+].[Na+]>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.O.C(COC)OC>[Br:14][C:15]1[CH:27]=[CH:26][C:25]2[C:24]3[C:19](=[CH:20][C:21]([C:2]4[CH:3]=[CH:4][C:5]5[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=5)[CH:1]=4)=[CH:22][CH:23]=3)[C:18]([CH3:30])([CH3:29])[C:17]=2[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

8

反応物 4

HCID 1140TolueneHCID 10340Sodium CarbonateHCID 2734375(Naphthalen-2-yl)boronic acidHCID 453821792-Bromo-7-iodo-9,9-dimethyl-9H-fluorene

生成物 1

HCID 576228742-bromo-9,9-dimethyl-7-(naphthalene-2-yl)-9H-fluorene収率 76.1%

試薬・触媒・溶媒 3

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

In argon atmosphere, a mixture of 13.91 g (80.9 mmol) of 2-naphthaleneboronic acid, 30.0 g (80.9 mmol) of 2-bromo-7-iodo-9,9-dimethylfluorene, 4.67 g (4.0 mmol) of tetrakis(triphenylphosphine)palladium (0), 200 ml of toluene, 200 ml of dimethoxyethane, and 122.36 g of a 2 M sodium carbonate aqueous solution was refluxed under stirring for 8 h and left standing overnight. After adding water, the mixture was stirred at room temperature for one hour. After filtration and extraction with toluene, the organic phase was washed with water and then with a saturated saline solution. After drying over sodium sulfate, the toluene was distilled off under reduced pressure. The residue was purified by silica gel chromatography to obtain 21.3 g (yield: 76.1%) of 2-bromo-9,9-dimethyl-7-(naphthalene-2-yl)-9H-fluorene.

後処理

  1. temperaturewas refluxed
  2. waitleft
  3. waitstanding overnight
  4. stirringthe mixture was stirred at room temperature for one hour
  5. filtrationAfter filtration and extraction with toluene
  6. washthe organic phase was washed with water
  7. dry with materialAfter drying over sodium sulfate
  8. distillationthe toluene was distilled off under reduced pressure
  9. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-28f40e28f10a42bb8e365ba43aea43bd
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08940412B2

反応ノート

読み込み中…

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