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Potassium Fluoride → Methyl 2'-methyl-2-(methylsulfonyl)biphenyl-4-carboxylate

HRID 219830
ノート
印刷プレビュー

反応式

HRID 219830 の反応式
Cl[C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[S:12]([CH3:15])(=[O:14])=[O:13].[C:16]1([CH3:25])[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1B(O)O.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.[F-].[K+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O.CO.C1(C)C=CC=CC=1>[CH3:25][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[S:12]([CH3:15])(=[O:14])=[O:13]
参加物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 522689Potassium FluorideHCID 27332672-Methylphenyl boronic acidHCID 10490815Methyl 4-chloro-3-(methylsulfonyl)benzoateHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl

生成物 1

HCID 67528382Methyl 2'-methyl-2-(methylsulfonyl)biphenyl-4-carboxylate収率 88.7%

試薬・触媒・溶媒 4

HCID 167845
palladium(II) acetate
触媒
HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

実験手順

In a schlenk flushed with Argon were added methyl 4-chloro-3-(methylsulfonyl)benzoate (124.34 mg; 0.50 mmol; 1 eq.), o-tolylboronic acid (84.97 mg; 0.62 mmol; 1.25 eq.), palladium(II) acetate (22.45 mg; 0.10 mmol; 0.20 eq.), 2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl (82.11 mg; 0.20 mmol; 0.40 eq.), potassium fluoride (87.14 mg; 1.50 mmol; 3 eq.), toluene (2.49 mL), MeOH (2.49 mL) and water (5.40 μl). The reaction was degassed with Ar and heated under reflux for 2 hours. Then, it was cooled down to RT. The solvents were evaporated and the crude mixture was dissolved in EtOAc, washed with water and brine and dried over MgSO4. The resulting crude product was purified by flash chromatography (c-hex/EtOAc 9:1 to 5:5), affording the title compound as a light yellow oil (135 mg; 88%). 1H NMR (DMSO-d6, 300 MHz) δ 8.89 (d, J=1.77 Hz, 1H), 8.32 (dd, J=1.77, 7.90 Hz, 1H), 7.43-7.19 (m, 5H), 4 (s, 3H), 2.76 (s, 3H), 2.09 (s, 3H). LC/MS (Method B): 305.1 (M+H)+. HPLC (max plot) 99.2%; Rt 4.51 min.

後処理

  1. customIn a schlenk flushed with Argon
  2. customThe reaction was degassed with Ar
  3. temperatureheated
  4. temperatureunder reflux for 2 hours
  5. customThe solvents were evaporated
  6. dissolutionthe crude mixture was dissolved in EtOAc
  7. washwashed with water and brine
  8. dry with materialdried over MgSO4
  9. customThe resulting crude product was purified by flash chromatography (c-hex/EtOAc 9:1 to 5:5)

出典と根拠

ORDレコード
ord-1f2d047105c649f6b7e09107e97eb42e
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08202865B2

反応ノート

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