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1H-1,2,4-Triazole → HCID 20079600, Verbindung

HRID 1033737
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1033737
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1([C:12]([S:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=2)([CH3:14])[CH3:13])[CH2:11][O:10]1.[NH:25]1[CH:29]=[N:28][CH:27]=[N:26]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:10])([C:12]([S:15][CH2:16][C:17]1[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=1)([CH3:14])[CH3:13])[CH2:11][N:25]1[CH:29]=[N:28][CH:27]=[N:26]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 19024387HCID 19024387, Verbindung

Produkt 1

HCID 20079600HCID 20079600, VerbindungAusbeute 94,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
105 °C

Versuchsvorschrift

A mixture of 64.0 g (182 mmol) of (-)-2-(2,4-difluorophenyl)-2-(1-((4-methoxyphenyl)methylthio)-1-methylethyl)oxirane, 25.1 g (364 mmol) of 1,2,4-triazole, 50.3 g (364 mmol) of potassium carbonate, and 910 ml of DMF was stirred at 105° C. for 17 hours. After allowing the mixture to cool, the solvent was removed by distillation under reduced pressure, and to the residue were added dichloromethane and water. The organic layer was separated, washed with a saturated sodium chloride aqueous solution, and dried. The solvent was removed by distillation under reduced pressure, and the residue was purified by column chromatography using a mixed solvent of chloroform and methanol (30:1) as an eluent. The solvent was removed by distillation under reduced pressure to obtain 72.0 g (94%) of (+)-2-(2,4-difluorophenyl)-3-((4-methoxyphenyl)methylthio)-3-methyl-1-(1H-1,2,4-triazol-1-yl)butan-2-ol as a pale yellow oily substance.

Aufarbeitung

  1. temperatureto cool
  2. customthe solvent was removed by distillation under reduced pressure
  3. additionto the residue were added dichloromethane and water
  4. customThe organic layer was separated
  5. washwashed with a saturated sodium chloride aqueous solution
  6. customdried
  7. customThe solvent was removed by distillation under reduced pressure
  8. customthe residue was purified by column chromatography
  9. customThe solvent was removed by distillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-af36e9d1059d41739aede6190f4d7d40
Quelldatensatz
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05312815

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