Lithium hydroxide, monohydrate → HCID 10665616, Verbindung

HRID 1108047Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1108047
C([O:4][CH2:5][CH2:6][S:7][C:8]([F:26])([F:25])[C:9]([C:17]1[CH:22]=[CH:21][C:20]([F:23])=[CH:19][C:18]=1[F:24])([OH:16])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1)(=O)C.O.[OH-].[Li+]>C(O)C>[F:24][C:18]1[CH:19]=[C:20]([F:23])[CH:21]=[CH:22][C:17]=1[C:9]([OH:16])([CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1)[C:8]([F:26])([F:25])[S:7][CH2:6][CH2:5][OH:4]

Komponenten

4

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 108343901-(2-acetoxyethyl)thio-2-(2,4-difluorophenyl)-1,1-difluoro-3-(1H-1,2,4-triazol-1-yl)propan-2-ol

Produkt 1

HCID 10665616HCID 10665616, VerbindungAusbeute 89,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of 1-(2-acetoxyethyl)thio-2-(2,4-difluorophenyl)-1,1-difluoro-3-(1H-1,2,4-triazol-1-yl)propan-2-ol (14.3 g, 0.12 mol) in ethanol (200 ml), a 10% aqueous solution (20 ml) of lithium hydroxide monohydrate was added and they were stirred at room temperature for one hour. After the completion of the reaction, the reaction mixture was distilled off under reduced pressure. Water was added to the residue so obtained, followed by extraction with chloroform. The chloroform solution was washed with water, dried over magnesium sulfate and then distilled off under reduced pressure, whereby 2-(2,4-difluorphenyl)-1,1-difluoro-1-(2-hydroxyethyl)thio-3-(1H-1,2,4-triazol-1-yl)propan-2-ol (11.4 g, yield: 89.8%) was obtained as colorless crystals.

Aufarbeitung

  1. customAfter the completion of the reaction
  2. distillationthe reaction mixture was distilled off under reduced pressure
  3. additionWater was added to the residue
  4. customso obtained
  5. extractionfollowed by extraction with chloroform
  6. washThe chloroform solution was washed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationdistilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9be61491f9804acfb06c9207fd0e3748
Quelldatensatz
uspto-grants-2000_05
Patentnummer
US06063945

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