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Toluene → 5-Formyl-4'-methylbiphenyl-3-carboxylic acid

HRID 1845339
ノート
印刷プレビュー

反応式

HRID 1845339 の反応式
Br[C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([CH:11]=[O:12])[CH:10]=1)[C:5]([OH:7])=[O:6].B(O)(O)[C:14]1[CH:15]=[CH:16][C:17]([CH3:20])=[CH:18][CH:19]=1.C1(C)C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+]>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>[CH:11]([C:9]1[CH:8]=[C:4]([C:5]([OH:7])=[O:6])[CH:3]=[C:2]([C:14]2[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=2)[CH:10]=1)=[O:12]
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 1140TolueneHCID 10796Cesium carbonateHCID 79799Tolylboronic acidHCID 223207963-Bromo-5-formylbenzoic acid

生成物 1

HCID 581880045-Formyl-4'-methylbiphenyl-3-carboxylic acid収率 57.2%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒

実験手順

To a mixture of 3-bromo-5-formylbenzoic acid (8.0 g, 34.9 mmol), p-tolylboronic acid (9.5 g, 70 mmol), toluene (300 mL), cesium carbonate (28 g, 87 mmol), and water (25 mL) under nitrogen was added tetrakis(triphenylphosphine)palladium(0) (2.0 g, 1.7 mmol). The mixture was heated under reflux for 5 h. After cooling, the mixture was filtered through Celite and the filter cake was washed with EtOAc. The filtrate was washed with brine, dried, and concentrated. The residue was purified by column chromatography using methylene chloride:methanol gradient (0-5%) to afford the title compound (4.8 g, 51%). LC-MS: 239.0 [M−1]−.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 5 h
  3. temperatureAfter cooling
  4. filtrationthe mixture was filtered through Celite
  5. washthe filter cake was washed with EtOAc
  6. washThe filtrate was washed with brine
  7. customdried
  8. concentrationconcentrated
  9. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-d264493ca37e4d6481c079debc6de78c
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946439B2

反応ノート

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