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Hydroxylamine HCl → 7-butyl-6-{[3,5-difluoro-2'-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}[1,2,4]triazolo[1,5-a]pyrimidin-5(4H)-one

HRID 519941
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HRID 519941 반응식
[Cl-].O[NH3+:3].[C:4](=[O:7])([O-])[OH:5].[Na+].[CH2:9]([C:13]1[N:18]2[N:19]=[CH:20][N:21]=[C:17]2[N:16](COC)[C:15](=[O:25])[C:14]=1[CH2:26][C:27]1[C:32]([F:33])=[CH:31][C:30]([C:34]2[C:35]([C:40]#[N:41])=[CH:36][CH:37]=[CH:38][CH:39]=2)=[CH:29][C:28]=1[F:42])[CH2:10][CH2:11][CH3:12].B(Br)(Br)Br>C(OCC)(=O)C.C(Cl)Cl.O.CS(C)=O>[CH2:9]([C:13]1[N:18]2[N:19]=[CH:20][N:21]=[C:17]2[NH:16][C:15](=[O:25])[C:14]=1[CH2:26][C:27]1[C:32]([F:33])=[CH:31][C:30]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=2[C:40]2[NH:3][C:4](=[O:7])[O:5][N:41]=2)=[CH:29][C:28]=1[F:42])[CH2:10][CH2:11][CH3:12]
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참가 물질

9

반응물 4

HCID 21645Hydroxylamine HClHCID 25134Boron tribromideHCID 516892Sodium BicarbonateHCID 670093794'-{[7-Butyl-4-(methoxymethyl)-5-oxo-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}-3',5'-difluorobiphenyl-2-carbonitrile

생성물 1

HCID 1360637287-butyl-6-{[3,5-difluoro-2'-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}[1,2,4]triazolo[1,5-a]pyrimidin-5(4H)-one
수율 7.2%

시약·촉매·용매 4

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매2회

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온도
40 °C

실험 절차

A mixture of hydroxylammonium chloride (0.87 g), sodium hydrogen carbonate (1.4 g) and dimethyl sulfoxide (10 mL) was stirred at 40° C. for 30 min, 4′-{[7-butyl-4-(methoxymethyl)-5-oxo-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}-3′,5′-difluorobiphenyl-2-carbonitrile (0.39 g) was added, and the mixture was stirred at 90° C. for 16 hr. The reaction mixture was diluted with ethyl acetate, washed with water and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was dissolved in tetrahydrofuran (10 mL). N,N′-Carbonyldiimidazole (0.16 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.14 mL) were added, and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with ethyl acetate, washed with saturated aqueous potassium hydrogensulfate solution and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue obtained by purification by silica gel column chromatography was dissolved in methylene chloride solution (10 mL), boron tribromide (1.0 M methylene chloride solution, 2.2 mL) was added, and the mixture was stirred at room temperature for 1 day. Ethyl acetate and water were added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was purified by silica gel column chromatography to give the title compound as colorless crystals (0.029 g, 7%).

후처리

  1. stirringthe mixture was stirred at 90° C. for 16 hr
  2. washwashed with water
  3. dry with materialwith saturated brine, and dried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. dissolutionthe residue was dissolved in tetrahydrofuran (10 mL)
  6. additionN,N′-Carbonyldiimidazole (0.16 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.14 mL) were added
  7. stirringthe mixture was stirred at room temperature for 2 hr
  8. additionThe reaction mixture was diluted with ethyl acetate
  9. washwashed with saturated aqueous potassium hydrogensulfate solution
  10. dry with materialwith saturated brine, and dried over anhydrous magnesium sulfate
  11. customThe solvent was evaporated under reduced pressure
  12. customThe residue obtained by purification by silica gel column chromatography
  13. stirringthe mixture was stirred at room temperature for 1 day
  14. extractionthe mixture was extracted with ethyl acetate
  15. washThe organic layer was washed with saturated brine
  16. dry with materialdried over anhydrous magnesium sulfate
  17. customthe solvent was evaporated
  18. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-441536a20c0c47d9b57a33787618c6ab
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115136B2

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