2-(2,4-Difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol → Hydrochloric Acid

HRID 1654229Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1654229
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C@:9]([OH:19])([C@H:16]([SH:18])[CH3:17])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1.[ClH:20].C(OCC)(=O)C>C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C@:9]([OH:19])([C@H:16]([SH:18])[CH3:17])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1.[ClH:20]

Komponenten

5

Edukt 2

HCID 1922642-(2,4-Difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol2×HCID 21866389Hydrogen chloride-ethyl acetate

Produkt 2

HCID 313Hydrochloric AcidHCID 1922642-(2,4-Difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

In ethyl acetate (10 ml) was dissolved (2R,3R)-2-(2,4-difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol (compound 43, 0.2 g) followed by addition of 4 N HCl-ethyl acetate (1 ml). The mixture was concentrated under reduced pressure to about 1 ml, whereupon crystals separated out. Then, ethyl ether (2 ml) was added and the mixture was filtered to give compound 43 hydrochloride (0.15 g) as colorless needles. m.p. 155°-162° C.

Aufarbeitung

  1. concentrationThe mixture was concentrated under reduced pressure to about 1 ml, whereupon crystals
  2. customseparated out
  3. additionThen, ethyl ether (2 ml) was added
  4. filtrationthe mixture was filtered

Quellen und Nachweise

ORD-Eintrag
ord-f211542f2d9a4498a090c0f2009934b7
Quelldatensatz
uspto-grants-1995_04
Patentnummer
US05405861

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