ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dimethyl Sulfoxide → 6-ethyl-3-[2-methoxy-2-(4-methoxyphenyl)ethyl]-1-{[2'-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione

HRID 1889487
ノート
印刷プレビュー

反応式

HRID 1889487 の反応式
[CH2:1]([C:3]1[S:39][C:6]2[N:7]([CH2:24][C:25]3[CH:30]=[CH:29][C:28]([C:31]4[C:32]([C:37]#[N:38])=[CH:33][CH:34]=[CH:35][CH:36]=4)=[CH:27][CH:26]=3)[C:8](=[O:23])[N:9]([CH2:12][C:13]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)=[O:14])[C:10](=[O:11])[C:5]=2[CH:4]=1)[CH3:2].[BH4-].[Na+].[Cl-].[OH:43][NH3+:44].[C:45](=[O:48])([O-])O.[Na+].[CH3:50]S(C)=O>C(Cl)(Cl)Cl.O1CCCC1>[CH2:1]([C:3]1[S:39][C:6]2[N:7]([CH2:24][C:25]3[CH:30]=[CH:29][C:28]([C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=4[C:37]4[NH:38][C:45](=[O:48])[O:43][N:44]=4)=[CH:27][CH:26]=3)[C:8](=[O:23])[N:9]([CH2:12][CH:13]([O:14][CH3:50])[C:15]3[CH:16]=[CH:17][C:18]([O:21][CH3:22])=[CH:19][CH:20]=3)[C:10](=[O:11])[C:5]=2[CH:4]=1)[CH3:2]
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 679Dimethyl Sulfoxide2 回HCID 21645Hydroxylamine HClHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 593515554'-{[6-ethyl-3-[2-(4-methoxyphenyl)-2-oxoethyl]-2,4-dioxo-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl]methyl}biphenyl-2-carbonitrile

生成物 1

HCID 136052323
6-ethyl-3-[2-methoxy-2-(4-methoxyphenyl)ethyl]-1-{[2'-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione
収率 36%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 4′-{[6-ethyl-3-[2-(4-methoxyphenyl)-2-oxoethyl]-2,4-dioxo-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl]methyl}biphenyl-2-carbonitrile (0.33 g) and tetrahydrofuran (20 mL) was added sodium borohydride (0.047 g), and the mixture was stirred at room temperature for 2 days. The reaction mixture was concentrated, and the residue was extracted with ethyl acetate and saturated aqueous ammonium chloride solution. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was dissolved in N,N-dimethylformamide (20 mL), sodium hydride (0.037 g) was added, and the mixture was stirred at room temperature for 10 min. Methyl iodide (0.046 mL) was added to the reaction mixture, and the mixture was further stirred at room temperature for 1 hr. The reaction mixture was diluted with ethyl acetate, washed successively with 5% aqueous potassium hydrogensulfate solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. To the obtained residue was added 1N aqueous sodium hydroxide solution (50 mL), and the mixture was stirred at 60° C. for 1 hr. The reaction mixture was adjusted to pH 4 with 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The obtained ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue obtained by silica gel column chromatography was dissolved in dimethyl sulfoxide (5 mL), and the mixture was added to a mixture of hydroxylammonium chloride (0.46 g), sodium hydrogencarbonate (0.7 g) and dimethyl sulfoxide (10 mL), which had been stirred at 40° C. for 30 min in advance. The reaction mixture was stirred at 90° C. for 16 hr, diluted with chloroform, washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was dissolved in methylene chloride (30 mL), N,N′-carbonyldiimidazole (0.068 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.057 mL) were added, and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with chloroform, washed successively with saturated aqueous potassium hydrogensulfate solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The precipitated solid was collected by filtration to give the title compound as colorless crystals (0.14 g, 36%).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. extractionthe residue was extracted with ethyl acetate and saturated aqueous ammonium chloride solution
  3. washThe ethyl acetate layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. dissolutionThe obtained residue was dissolved in N,N-dimethylformamide (20 mL)
  7. additionsodium hydride (0.037 g) was added
  8. stirringthe mixture was stirred at room temperature for 10 min
  9. additionMethyl iodide (0.046 mL) was added to the reaction mixture
  10. stirringthe mixture was further stirred at room temperature for 1 hr
  11. additionThe reaction mixture was diluted with ethyl acetate
  12. washwashed successively with 5% aqueous potassium hydrogensulfate solution and saturated brine
  13. dry with materialdried over anhydrous magnesium sulfate
  14. customThe solvent was evaporated under reduced pressure
  15. additionTo the obtained residue was added 1N aqueous sodium hydroxide solution (50 mL)
  16. stirringthe mixture was stirred at 60° C. for 1 hr
  17. extractionthe mixture was extracted with ethyl acetate
  18. washThe obtained ethyl acetate layer was washed with saturated brine
  19. dry with materialdried over anhydrous magnesium sulfate
  20. customThe solvent was evaporated under reduced pressure
  21. customThe residue obtained by silica gel column chromatography
  22. stirringhad been stirred at 40° C. for 30 min in advance
  23. stirringThe reaction mixture was stirred at 90° C. for 16 hr
  24. washwashed successively with water and saturated brine
  25. dry with materialdried over anhydrous magnesium sulfate
  26. customThe solvent was evaporated under reduced pressure
  27. dissolutionThe residue was dissolved in methylene chloride (30 mL)
  28. additionN,N′-carbonyldiimidazole (0.068 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.057 mL) were added
  29. stirringthe mixture was stirred at room temperature for 2 hr
  30. additionThe reaction mixture was diluted with chloroform
  31. washwashed successively with saturated aqueous potassium hydrogensulfate solution and saturated brine
  32. dry with materialdried over anhydrous magnesium sulfate
  33. customThe solvent was evaporated under reduced pressure
  34. filtrationThe precipitated solid was collected by filtration

出典と根拠

ORDレコード
ord-01f87c4b3a1f4fc08edb1f6a64ab4774
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501750B2

反応ノート

読み込み中…

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