Hydrogen chloride-ethyl acetate → (2R,3R)-2-(2,4-Difluorophenyl)-3-(1H-1,2,4-triazol-1-yl)-3-[(piperidin-4-yl)thio]-2-butanol dihydrochloride

HRID 379936

Reaktionsgleichung

Reaktionsgleichung von HRID 379936
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C@@:9]([OH:32])([C@:11]([N:27]1[CH:31]=[N:30][CH:29]=[N:28]1)([S:13][CH:14]1[CH2:19][CH2:18][N:17](C(OC(C)(C)C)=O)[CH2:16][CH2:15]1)[CH3:12])[CH3:10].C(OCC)(=O)C.[ClH:39]>C(OCC)(=O)C>[ClH:39].[ClH:39].[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C@@:9]([OH:32])([C@:11]([N:27]1[CH:31]=[N:30][CH:29]=[N:28]1)([S:13][CH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1)[CH3:12])[CH3:10]

Komponenten

4

Edukt 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 53773004(2R,3R)-2-(2,4-Difluorophenyl)-3-(1H-1,2,4-triazol-1-yl)-3-[[1-(tert-butoxycarbonyl)piperidin-4-yl]thio]-2-butanol

Produkt 1

HCID 70196509(2R,3R)-2-(2,4-Difluorophenyl)-3-(1H-1,2,4-triazol-1-yl)-3-[(piperidin-4-yl)thio]-2-butanol dihydrochlorideAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

In 20 ml of ethyl acetate were dissolved 557 mg (1.05 mmol) of (2R,3R)-2-(2,4-difluorophenyl)-3-(1H-1,2,4-triazol-1-yl)-3-[[1-(tert-butoxycarbonyl)piperidin-4-yl]thio]-2-butanol, and 2.63 ml (10.5 mmol) of a 4N hydrogen chloride-ethyl acetate solution were added to the solution, followed by stirring of the resulting mixture at 40° C. for 8 hours. After cooling, the precipitated solid was collected by filtration and washed with hexane to obtain 460 mg (yield: 100%) of the desired compound as a colorless powder.

Aufarbeitung

  1. additionwere added to the solution
  2. temperatureAfter cooling
  3. filtrationthe precipitated solid was collected by filtration
  4. washwashed with hexane

Quellen und Nachweise

ORD-Eintrag
ord-59971445f4f244448b7d7d12bc182f9f
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06300357B1

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