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Tetrahydrofuran → HCID 178438770, Verbindung

HRID 1688623
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1688623
[Si]([O:8][CH:9]1[CH2:14][CH2:13][CH:12]([N:15]2[C:20](=[O:21])[C:19]([CH2:22][C:23]3[CH:24]=[CH:25][C:26]([C:29]4[CH:36]=[CH:35][CH:34]=[CH:33][C:30]=4[C:31]#[N:32])=[N:27][CH:28]=3)=[C:18]([CH2:37][CH2:38][CH3:39])[N:17]3[N:40]=[CH:41][N:42]=[C:16]23)[CH2:11][CH2:10]1)(C(C)(C)C)(C)C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCCC1.[C:66]([O:69][CH2:70][CH3:71])(=[O:68])[CH3:67]>O>[C:31]([C:30]1[CH:33]=[CH:34][CH:35]=[CH:36][C:29]=1[C:26]1[N:27]=[CH:28][C:23]([CH2:22][C:19]2[C:20](=[O:21])[N:15]([C@H:12]3[CH2:13][CH2:14][C@H:9]([O:8][CH2:67][C:66]([O:69][CH2:70][CH3:71])=[O:68])[CH2:10][CH2:11]3)[C:16]3[N:17]([N:40]=[CH:41][N:42]=3)[C:18]=2[CH2:37][CH2:38][CH3:39])=[CH:24][CH:25]=1)#[N:32]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8028TetrahydrofuranHCID 8857Ethyl AcetateHCID 2724141Tetrabutylammonium FluorideHCID 670092682-(5-{[4-(4-{[Tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}pyridin-2-yl)benzonitrile

Produkt 1

HCID 178438770HCID 178438770, VerbindungAusbeute 15 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture of 2-(5-{[4-(4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}pyridin-2-yl)benzonitrile (0.42 g), tetrabutylammonium fluoride (1 M tetrahydrofuran solution, 1.1 mL) and tetrahydrofuran (20 mL) was stirred at 70° C. for 16 hr. Ethyl acetate and water were added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was dissolved in acetonitrile (20 mL), 1,1,1-triacetoxy-1,1-dihydro-1,2-benziodoxol-3(1H)-one (0.31 g) was added, and the mixture was stirred at room temperature for 3 hr. Saturated aqueous sodium hydrogen carbonate solution and sodium thiosulfate were added to the reaction mixture, and the mixture was stirred at room temperature for 2 hr, and extracted with ethyl acetate. The organic 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 tetrahydrofuran (3 mL) and methanol (3 mL), sodium borohydride (0.016 g) was added, and the mixture was stirred at room temperature for 1 hr. After evaporation of the solvent under reduced pressure, the residue was extracted with water and 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. To a solution (10 mL) of the obtained residue in toluene was added dropwise ethyl diazoacetate (0.14 mL) in the presence of rhodium(I) acetate (0.0012 g) at 80° C., and the mixture was stirred at the same temperature for 1 hr. The reaction mixture was concentrated, and the obtained residue was subjected to silica gel column chromatography to give the title compound as a colorless solid (0.06 g, 15%).

Aufarbeitung

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialwith saturated brine, and dried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. dissolutionThe obtained residue was dissolved in acetonitrile (20 mL)
  6. addition1,1,1-triacetoxy-1,1-dihydro-1,2-benziodoxol-3(1H)-one (0.31 g) was added
  7. stirringthe mixture was stirred at room temperature for 3 hr
  8. additionSaturated aqueous sodium hydrogen carbonate solution and sodium thiosulfate were added to the reaction mixture
  9. stirringthe mixture was stirred at room temperature for 2 hr
  10. extractionextracted with ethyl acetate
  11. washThe organic layer was washed with saturated brine
  12. dry with materialdried over anhydrous magnesium sulfate
  13. customThe solvent was evaporated under reduced pressure
  14. dissolutionThe obtained residue was dissolved in tetrahydrofuran (3 mL)
  15. additionmethanol (3 mL), sodium borohydride (0.016 g) was added
  16. stirringthe mixture was stirred at room temperature for 1 hr
  17. customAfter evaporation of the solvent under reduced pressure
  18. extractionthe residue was extracted with water and ethyl acetate
  19. washThe obtained ethyl acetate layer was washed with saturated brine
  20. dry with materialdried over anhydrous magnesium sulfate
  21. customThe solvent was evaporated under reduced pressure
  22. additionTo a solution (10 mL) of the obtained residue in toluene was added dropwise ethyl diazoacetate (0.14 mL) in the presence of rhodium(I) acetate (0.0012 g) at 80° C.
  23. stirringthe mixture was stirred at the same temperature for 1 hr
  24. concentrationThe reaction mixture was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-9f1d6d3edf3d4165b0f0e3d3b34d1c56
Quelldatensatz
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08148383B2

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