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Sodium Carbonate → Ethyl 2'-fluoro-4-hydroxy-5'-methoxy-[1,1'-biphenyl]-2-carboxylate

HRID 1049504
ノート
印刷プレビュー

反応式

HRID 1049504 の反応式
Br[C:2]1[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5].[F:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][C:16]=1B(O)O.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.O.Cl.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[F:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][C:16]=1[C:2]1[C:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])=[CH:9][C:10]([OH:13])=[CH:11][CH:12]=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

9

反応物 4

HCID 10340Sodium CarbonateHCID 41572112-Fluoro-5-methoxyphenylboronic acidHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 53487920Ethyl 2-bromo-5-hydroxybenzoate

生成物 1

HCID 117759944Ethyl 2'-fluoro-4-hydroxy-5'-methoxy-[1,1'-biphenyl]-2-carboxylate収率 103.1%

試薬・触媒・溶媒 4

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 313Hydrochloric Acid溶媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

Under an argon atmosphere, to a solution of ethyl 2-bromo-5-hydroxybenzoate (1.13 g) in toluene (30 mL) were added 2-fluoro-5-methoxyphenylboronic acid (1.18 g), 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (379 mg), 75% tris(dibenzylideneacetone)dipalladium (0) (281 mg) and 2.0 M aqueous sodium carbonate solution (6.9 mL), and the mixture was stirred at 100° C. for 21.5 hr. The reaction mixture was diluted with water and 1N hydrochloric acid, and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (1.38 g) as a pale-yellow oil.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-ee6a8bd2a1ee4ebf87d9057fc08928d9
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09382188B2

反応ノート

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