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Potassium Carbonate → 6-(4-Methoxyphenyl)-2-pyridinecarbonitrile

HRID 748276
ノート
印刷プレビュー

反応式

HRID 748276 の反応式
Cl[C:2]1[N:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][CH:3]=1.[CH3:10][O:11][C:12]1[CH:17]=[CH:16][C:15](OB(O)O)=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.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.O.C(OCC)(=O)C>[CH3:10][O:11][C:12]1[CH:17]=[CH:16][C:15]([C:2]2[N:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][CH:3]=2)=[CH:14][CH:13]=1
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 3

HCID 11430Potassium CarbonateHCID 1184246-Chloropyridine-2-carbonitrileHCID 147699944-Methoxyphenyl boric acid

生成物 1

HCID 229396246-(4-Methoxyphenyl)-2-pyridinecarbonitrile収率 89.4%

試薬・触媒・溶媒 5

HCID 178418397HCID 178418397、化合物触媒
HCID 702
Ethanol
溶媒
HCID 962Water溶媒2 回
HCID 1140Toluene溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

6-Chloro-2-pyridinecarbonitrile (0.70 g, 5.0 mmol) and 4-methoxyphenylboric acid (1.17 g, 7.7 mmol) were dissolved in toluene (60 ml)-ethanol (15 ml), and potassium carbonate (1.75 g, 12.6 mmol) and water (15 ml) were added thereto. The mixture was deairated under reduced pressure for 10 minutes. Tetrakis(triphenylphosphine)palladium (0) (0.29 g, 0.25 mmol) was added to the reaction mixture under argon atmosphere, and the mixture was refluxed for 16 hrs. The reaction mixture was combined with ethyl acetate and water. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with hexane-ethyl acetate (4:1, v/v) were collected, concentrated and recrystallized from hexane-ethyl acetate to give the titled compound (0.94 g, 88%).

後処理

  1. additionwere added
  2. temperaturethe mixture was refluxed for 16 hrs
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. washThe fractions eluted with hexane-ethyl acetate (4:1
  7. customv/v) were collected
  8. concentrationconcentrated
  9. customrecrystallized from hexane-ethyl acetate

出典と根拠

ORDレコード
ord-4280ba253fb141f296b5075796121126
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07399759B2

反応ノート

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