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Potassium Hydroxide → HCID 68157225、化合物

HRID 243073
ノート
印刷プレビュー

反応式

HRID 243073 の反応式
[Br:1][C:2]1[C:7](F)=[CH:6][CH:5]=[C:4]([N+:9]([O-:11])=[O:10])[C:3]=1[NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(P(C(C)(C)C)C1C=CC=CC=1C1C(C(C)C)=CC(C(C)C)=CC=1C(C)C)(C)(C)C.[OH-:49].[K+]>O1CCOCC1.O.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]>[Br:1][C:2]1[C:3]([NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1[OH:49]
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 3

HCID 14797Potassium HydroxideHCID 11618717Di-tert-butyl(2',4',6'-tris(propan-2-yl)-(1,1'-biphenyl)-2-yl)phosphaneHCID 68157998(2-Bromo-3-fluoro-6-nitrophenyl)phenylamine

生成物 1

HCID 68157225HCID 68157225、化合物収率 59.2%

試薬・触媒・溶媒 3

HCID 9811564Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
90 °C

実験手順

To a solution of (2-bromo-3-fluoro-6-nitrophenyl)phenylamine (1.5 g, 4.8 mmol) in dioxane (20 mL) and water (10 mL) was added tris(dibenzylideneacetone)dipalladium (0) (88 mg, 0.96 mmol), 2-di-tert-butylphosphino-2′,4′,6′-triisopropylbiphenyl (164 mg, 0.39 mmol) and potassium hydroxide (812 mg, 14.4 mmol). The reaction mixture was degassed by bubbling argon through the mixture whilst undergoing sonication. The reaction mixture was heated at 90° C. for 3 h before being diluted with water and acidified to ˜pH 3 by addition of HCl (1N). The mixture was extracted with EtOAc (3×20 mL). The combined organic fractions were washed with brine, dried (MgSO4), concentrated in vacuo and the resultant residue subjected to flash chromatography (SiO2, eluting with 0-100% EtOAc in cyclohexane) to give the title compound as a yellow solid (879 mg, 59%). 1H NMR 400 MHz 6 (CDCl3): 8.85 (1H, br s), 8.18 (1H, d, J=12.6 Hz), 7.31-7.24 (2H, m), 7.10-7.03 (1H, m), 6.92-6.86 (2H, m), 6.80 (1H, d, J=12.6 Hz).

後処理

  1. customThe reaction mixture was degassed
  2. customby bubbling argon through the mixture
  3. customsonication
  4. additionbefore being diluted with water
  5. additionby addition of HCl (1N)
  6. extractionThe mixture was extracted with EtOAc (3×20 mL)
  7. washThe combined organic fractions were washed with brine
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated in vacuo
  10. washthe resultant residue subjected to flash chromatography (SiO2, eluting with 0-100% EtOAc in cyclohexane)

出典と根拠

ORDレコード
ord-5239ba6e7aa14396b1cae36d7dc972f7
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08653089B2

反応ノート

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