Lithium Hydroxide → HCID 58277349, Verbindung

HRID 1949261Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1949261
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[CH:14]=3)=[CH:11][C:10]([C:20]([O:22]CC)=[O:21])=[N:9]2)=[CH:4][CH:3]=1.[OH-].[Li+]>O1CCOCC1.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[CH:14]=3)=[CH:11][C:10]([C:20]([OH:22])=[O:21])=[N:9]2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 2

HCID 3939Lithium HydroxideHCID 58277374HCID 58277374, Verbindung

Produkt 1

HCID 58277349HCID 58277349, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

43.0 g (125 mmol) of the compound of Example 56A are provided in 504 ml of 1,4-dioxane, 94 ml (188 mmol) of a 2N solution of lithium hydroxide in water are added, and the mixture is stirred at 70° C. for 2 h. The mixture is concentrated, a conc. aqueous hydrogen chloride solution is subsequently added to the residue until the pH is acidic, the mixture is extracted with dichloromethane, and the organic phase is dried over magnesium sulfate, filtered and concentrated. 39.5 g (100% of theory) of the title compound are obtained.

Aufarbeitung

  1. concentrationThe mixture is concentrated
  2. additiona conc. aqueous hydrogen chloride solution is subsequently added to the residue until the pH
  3. extractionthe mixture is extracted with dichloromethane
  4. dry with materialthe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-5764eda8dbbf4ced87049dba07f69fa6
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08399682B2

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