Hydrochloric Acid → HCID 57742536, Verbindung

HRID 2266491Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2266491
C[O:2][C:3](=[O:30])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]2[C:7]=1[C:8]([CH3:29])=[C:9]([CH2:21][C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=1)[C:10]([O:17][CH:18]([F:20])[F:19])=[N:11]2.O1CCCC1.[OH-].[Li+].Cl>CO>[Cl:28][C:25]1[CH:24]=[CH:23][C:22]([CH2:21][C:9]2[C:10]([O:17][CH:18]([F:19])[F:20])=[N:11][C:12]3[C:7]([C:8]=2[CH3:29])=[C:6]([O:5][CH2:4][C:3]([OH:30])=[O:2])[CH:15]=[CH:14][C:13]=3[F:16])=[CH:27][CH:26]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 68785003HCID 68785003, Verbindung

Produkt 1

HCID 57742536HCID 57742536, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of [3-(4-chlorobenzyl)-2-difluoromethoxy-8-fluoro-4-methylquinolin-5-yloxy]acetic acid methyl ester (0.45 g), tetrahydrofuran (5.0 mL), methanol (5.0 mL) and 1.0 M aqueous lithium hydroxide solution (1.3 mL) was stirred at room temperature for 18 hours. The solution was acidified by the addition of 1.0 M aqueous hydrochloric acid and extracted with ethyl acetate. The combined extracts were dried over magnesium sulfate and the solvent removed under reduced pressure. Crystallisation of the residue from a mixture of water and propan-2-ol gave title compound as a white solid, 0.33 g.

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined extracts were dried over magnesium sulfate
  3. customthe solvent removed under reduced pressure
  4. customCrystallisation of the residue
  5. additionfrom a mixture of water and propan-2-ol

Quellen und Nachweise

ORD-Eintrag
ord-f5cbb573ff4b4a3d8bf523c5985d8d11
Quelldatensatz
uspto-grants-2010_12
Patentnummer
US07858640B2

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