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Dimethylformamide → 5-(3,4-Difluorophenyl)-2,3-dimethyl-benzoic acid

HRID 1771817
ノート
印刷プレビュー

反応式

HRID 1771817 の反応式
Br[C:2]1[CH:3]=[C:4]([CH3:12])[C:5]([CH3:11])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].[F:13][C:14]1[CH:15]=[C:16](B(O)O)[CH:17]=[CH:18][C:19]=1[F:20].C([O-])([O-])=O.[Na+].[Na+].CN(C=O)C>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.O>[F:13][C:14]1[CH:15]=[C:16]([C:2]2[CH:3]=[C:4]([CH3:12])[C:5]([CH3:11])=[C:6]([CH:10]=2)[C:7]([OH:9])=[O:8])[CH:17]=[CH:18][C:19]=1[F:20]
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

8

反応物 4

HCID 6228DimethylformamideHCID 10340Sodium CarbonateHCID 27343373,4-Difluorobenzeneboronic acidHCID 668959895-Bromo-2,3-dimethylbenzoic acid

生成物 1

HCID 894452845-(3,4-Difluorophenyl)-2,3-dimethyl-benzoic acid収率 70%

試薬・触媒・溶媒 3

HCID 178418397
HCID 178418397、化合物
触媒
HCID 702Ethanol溶媒
HCID 962Water溶媒2 回

反応条件

温度
100 °C

実験手順

To a mixture of 5-bromo-2,3-dimethyl-benzoic acid (500 mg, 2.18 mmol, 1.0 eq), (3,4-difluorophenyl)boronic acid (378.6 mg, 2.40 mmol, 1.1 eq) and Na2CO3 (693 mg, 6.54 mmol, 3.0 eq) in a mixture of EtOH (2.5 mL), DMF (10 mL) and H2O (2.5 mL) was added Pd(PPh3)4 (126 mg, 0.11 mmol, 0.05 eq) under nitrogen. The mixture was stirred at 100° C. overnight. After cooling to room temperature, water was added and the diluted reaction mixture filtered through celite. The aqueous layer was extracted with EtOAc and the organic extract was discarded. The remaining aqueous layer was acidified to pH 2 by addition of 3M HCl. The resulting mixture was extracted with EtOAc and the combined organic extracts were washed with water and brine, dried (Na2SO4), filtered and evaporated in vacuo to give the title compound as a white solid (400 mg, 70%).

後処理

  1. temperatureAfter cooling to room temperature
  2. customthe diluted reaction mixture
  3. filtrationfiltered through celite
  4. extractionThe aqueous layer was extracted with EtOAc
  5. extractionthe organic extract
  6. additionThe remaining aqueous layer was acidified to pH 2 by addition of 3M HCl
  7. extractionThe resulting mixture was extracted with EtOAc
  8. washthe combined organic extracts were washed with water and brine
  9. dry with materialdried (Na2SO4)
  10. filtrationfiltered
  11. customevaporated in vacuo

出典と根拠

ORDレコード
ord-3415f8a2e6b6415c8fabd44d6304c278
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09249085B2

反応ノート

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