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Pyridine → 3-(4-isopropoxyphenyl)-5-{[2-methoxy-2'-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}-2-methyl-6-propylpyrimidin-4(3H)-one

HRID 1718923
ノート
印刷プレビュー

反応式

HRID 1718923 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH2:9][C:10]2[C:15](=[O:16])[NH:14][C:13]([CH3:17])=[N:12][C:11]=2[CH2:18][CH2:19][CH3:20])[CH:6]=[CH:5][C:4]=1[C:21]1[C:22]([C:27]#[N:28])=[CH:23][CH:24]=[CH:25][CH:26]=1.[CH:29]([O:32][C:33]1[CH:38]=[CH:37][C:36](B(O)O)=[CH:35][CH:34]=1)([CH3:31])[CH3:30].C([N:44](CC)CC)C.N1C=CC=CC=1.[C:55]([O:58]CC)(=[O:57])C>ClCCl.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[CH:29]([O:32][C:33]1[CH:38]=[CH:37][C:36]([N:14]2[C:15](=[O:16])[C:10]([CH2:9][C:7]3[CH:6]=[CH:5][C:4]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[C:27]4[NH:44][C:55](=[O:57])[O:58][N:28]=4)=[C:3]([O:2][CH3:1])[CH:8]=3)=[C:11]([CH2:18][CH2:19][CH3:20])[N:12]=[C:13]2[CH3:17])=[CH:35][CH:34]=1)([CH3:31])[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 1049PyridineHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 36987264-Isopropoxybenzeneboronic acidHCID 1361468682'-Methoxy-4'-[(2-methyl-6-oxo-4-propyl-1,6-dihydropyrimidin-5-yl)methyl]biphenyl-2-carbonitrile

生成物 1

HCID 136146780
3-(4-isopropoxyphenyl)-5-{[2-methoxy-2'-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}-2-methyl-6-propylpyrimidin-4(3H)-one
収率 58%

試薬・触媒・溶媒 2

HCID 8895Cupric acetate触媒HCID 6344Dichloromethane溶媒

実験手順

To a suspension of 2′-methoxy-4′-[(2-methyl-6-oxo-4-propyl-1,6-dihydropyrimidin-5-yl)methyl]biphenyl-2-carbonitrile (1.00 g), (4-isopropoxyphenyl)boronic acid (1.00 g), triethylamine (1.3 mL), pyridine (2.5 mL) and molecular sieves 4 A (2.50 g) in dichloromethane (30 mL) was added copper(II) acetate (0.98 g) and the mixture was stirred at room temperature for 2 days. The reaction mixture was diluted with ethyl acetate, the insoluble material was filtered off through celite, and the filtrate was concentrated. The residue was purified by silica gel column chromatography. The crudely purified product was added to a mixture of hydroxylammonium chloride (2.05 g), sodium hydrogen carbonate (3.31 g) and dimethyl sulfoxide (10 mL), which had been stirred at 40° C. for 30 min, and the mixture was stirred at 90° C. for 18 hr. The reaction mixture was allowed to cool to room temperature, ethyl acetate and water were added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated and the residue was dissolved in tetrahydrofuran (10 mL). N,N′-carbonyldiimidazole (0.48 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.45 mL) were added, and the mixture was stirred at room temperature for 3 hr. The reaction mixture was diluted with ethyl acetate, washed with 1 M hydrochloric acid and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography to give the title compound as colorless crystals (0.88 g, 58%).

後処理

  1. filtrationthe insoluble material was filtered off through celite
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by silica gel column chromatography
  4. additionThe crudely purified product was added to a mixture of hydroxylammonium chloride (2.05 g), sodium hydrogen carbonate (3.31 g) and dimethyl sulfoxide (10 mL), which
  5. stirringhad been stirred at 40° C. for 30 min
  6. stirringthe mixture was stirred at 90° C. for 18 hr
  7. temperatureto cool to room temperature
  8. additionethyl acetate and water were added
  9. extractionthe mixture was extracted with ethyl acetate
  10. washThe organic layer was washed with saturated brine
  11. dry with materialdried over anhydrous magnesium sulfate
  12. customThe solvent was evaporated
  13. dissolutionthe residue was dissolved in tetrahydrofuran (10 mL)
  14. additionN,N′-carbonyldiimidazole (0.48 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.45 mL) were added
  15. stirringthe mixture was stirred at room temperature for 3 hr
  16. additionThe reaction mixture was diluted with ethyl acetate
  17. washwashed with 1 M hydrochloric acid
  18. dry with materialwith saturated brine, and dried over anhydrous magnesium sulfate
  19. customThe solvent was evaporated under reduced pressure
  20. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-988fdc92a6244941a05a6cf767ee6649
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07803940B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート