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Hydrogen Bromide → (8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyridine dihydrobromide

HRID 2369351
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2369351
[BrH:1].[CH3:2][O:3][C:4]1[N:9]=[C:8](/[CH:10]=[CH:11]/[C:12]2[N:30]=[C:15]3[C@H:16]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=4[C:26]([F:29])([F:28])[F:27])[CH2:17][CH2:18][CH2:19][N:14]3[N:13]=2)[CH:7]=[CH:6][C:5]=1[N:31]1[CH:35]=[C:34]([CH3:36])[N:33]=[CH:32]1.CCCCCCC>C(O)C>[BrH:1].[BrH:1].[CH3:2][O:3][C:4]1[N:9]=[C:8](/[CH:10]=[CH:11]/[C:12]2[N:30]=[C:15]3[C@H:16]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=4[C:26]([F:29])([F:28])[F:27])[CH2:17][CH2:18][CH2:19][N:14]3[N:13]=2)[CH:7]=[CH:6][C:5]=1[N:31]1[CH:35]=[C:34]([CH3:36])[N:33]=[CH:32]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 260Hydrogen BromideHCID 8900Heptane2×HCID 46854987E-2212

Produkt 1

HCID 66991574(8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyridine dihydrobromide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702
Ethanol
Lösungsmittel

Versuchsvorschrift

Concentrated hydrobromic acid (24.8 μL) was added to a solution of (8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyridine (51.42 mg) in ethanol (1 mL), and 1 mL of heptane was added with stirring at room temperature. After several minutes, 1 mL of heptane was further added to the solution and stirring was continued. The solution was stirred at room temperature for one hour and then further stirred at about 5° C. for 20 minutes. The precipitated solid was collected by filtration through a glass filter and dried under reduced pressure at room temperature to obtain 49.24 mg of the title compound as white solid crystals.

Aufarbeitung

  1. additionwas added
  2. waitAfter several minutes
  3. stirringstirring
  4. stirringThe solution was stirred at room temperature for one hour
  5. stirringfurther stirred at about 5° C. for 20 minutes
  6. filtrationThe precipitated solid was collected by filtration through a glass
  7. filtrationfilter
  8. customdried under reduced pressure at room temperature

Quellen und Nachweise

ORD-Eintrag
ord-4ff0de4d925a419daa5a0c4a91cb4f8b
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08703954B2

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