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Ethanol → 3',4-Difluoro-[1,1'-biphenyl]-3-carboxylic acid

HRID 1528010
ノート
印刷プレビュー

反応式

HRID 1528010 の反応式
[F:1][C:2]1[CH:3]=[C:4](B(O)O)[CH:5]=[CH:6][CH:7]=1.Br[C:12]1[CH:13]=[CH:14][C:15]([F:21])=[C:16]([CH:20]=1)[C:17]([OH:19])=[O:18].C(=O)([O-])[O-].[Cs+].[Cs+].C(O)C>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.C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[C:4]([C:12]2[CH:13]=[CH:14][C:15]([F:21])=[C:16]([C:17]([OH:19])=[O:18])[CH:20]=2)[CH:5]=[CH:6][CH:7]=1
参加物反応条件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 702EthanolHCID 10796Cesium carbonateHCID 27339863-Fluorophenylboronic acidHCID 27363155-Bromo-2-fluorobenzoic acid

生成物 1

HCID 463123323',4-Difluoro-[1,1'-biphenyl]-3-carboxylic acid

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

A 50 mL Schlenk tube was charged with (3-fluorophenyl)boronic acid (140 mg, 1.0 mmol), 5-bromo-2-fluorobenzoic acid (263 mg, 1.2 mmol), tetrakis(triphenylphosphine)palladium (0) (58 mg, 0.05 mmol) and cesium carbonate (1.3 g, 4.0 mmol). Ethanol (5 mL) and toluene (5 mL) were added and the tube was sealed and heated at 80° C. for 3 h. The cooled mixture was transferred to a flask, washing with ethanol, and concentrated in vacuo. The residue was diluted with water (10 mL) and extracted with EtOAc (2×10 mL). The aqueous phase was acidified with 1.0 N aqueous HCl (10 mL) and extracted with EtOAc (3×10 mL). The extracts were dried (Na2SO4), filtered and concentrated in vacuo. 1H-NMR showed the desired product, 3′,4-difluoro-[1,1′-biphenyl]-3-carboxylic acid, was slightly contaminated with 2-fluorobenzoic acid. The impure product (215 mg, ˜92%) was used without further purification.

後処理

  1. customthe tube was sealed
  2. customThe cooled mixture was transferred to a flask
  3. washwashing with ethanol
  4. concentrationconcentrated in vacuo
  5. additionThe residue was diluted with water (10 mL)
  6. extractionextracted with EtOAc (2×10 mL)
  7. extractionextracted with EtOAc (3×10 mL)
  8. dry with materialThe extracts were dried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customThe impure product (215 mg, ˜92%) was used without further purification

出典と根拠

ORDレコード
ord-e17ba03d914e4f2489dd1bc8a3cd1a26
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090584B2

反応ノート

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