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Sodium Carbonate → 3-(5-Ethyl-2-methyl-6-oxo-1,6-dihydropyridin-3-yl)benzonitrile

HRID 1921317
ノート
印刷プレビュー

反応式

HRID 1921317 の反応式
Br[C:2]1[CH:3]=[C:4]([CH2:10][CH3:11])[C:5](=[O:9])[NH:6][C:7]=1[CH3:8].[C:12]([C:14]1[CH:15]=[C:16](B(O)O)[CH:17]=[CH:18][CH:19]=1)#[N:13].C(=O)([O-])[O-].[Na+].[Na+]>C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Pd].C1(C)C=CC=CC=1>[CH2:10]([C:4]1[C:5](=[O:9])[NH:6][C:7]([CH3:8])=[C:2]([C:18]2[CH:19]=[C:14]([CH:15]=[CH:16][CH:17]=2)[C:12]#[N:13])[CH:3]=1)[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 27343253-Cyanophenylboronic acidHCID 207792745-bromo-3-ethyl-6-methyl-1H-pyridin-2-one

生成物 1

HCID 116300653-(5-Ethyl-2-methyl-6-oxo-1,6-dihydropyridin-3-yl)benzonitrile収率 36%

試薬・触媒・溶媒 2

HCID 11979704Tetrakis(triphenylphosphine)palladium触媒
HCID 1140Toluene溶媒

実験手順

A stirred mixture of 5-bromo-3-ethyl-6-methyl-1H-pyridin-2-one, prepared in accordance with the procedures of PREPARATION 1, Step 2, (100 mg, 0.46 mmol), 3-cyanophenylboronic acid (88 mg, 0.6 mmol), 2M aq sodium carbonate (0.69 mL, 1.38 mmol), palladium tetrakis(triphenylphosphine) (16 mg, 0.014 mmol) and toluene (5 mL) is heated at reflux under a nitrogen atmosphere. After 2 hr, more catalyst (16 mg) is added and heating is continued overnight. The reaction is cooled and the mixture is partitioned between water and dichloromethane. The organic layer is separated and the solvents are removed. The residue is purified by chromatography eluting with ethyl acetate and with dichloromethane-5% methanol. Fractions containing product are combined, concentrated and the residue is triturated with hot ether to afford 3-(5-ethyl-2-methyl-6-oxo-1,6-dihydropyridin-3-yl)benzonitrile (40 mg, 36%) as a white solid. LC/MS: MS m/e=239 (M+H); RT 2.83 min.

後処理

  1. temperatureis heated
  2. temperatureat reflux under a nitrogen atmosphere
  3. temperatureheating
  4. waitis continued overnight
  5. temperatureThe reaction is cooled
  6. customthe mixture is partitioned between water and dichloromethane
  7. customThe organic layer is separated
  8. customthe solvents are removed
  9. customThe residue is purified by chromatography
  10. washeluting with ethyl acetate and with dichloromethane-5% methanol
  11. additionFractions containing product
  12. concentrationconcentrated
  13. customthe residue is triturated with hot ether

出典と根拠

ORDレコード
ord-b129b93d2bf245c28e7122e626a47e52
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08173682B2

反応ノート

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