Hydrochloric Acid → HCID 22251491, Verbindung

HRID 1264354Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1264354
C[O:2][C:3](=[O:20])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][C:12](=[O:19])[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:6][CH:5]=1.[Li+].[OH-].Cl>O.C1COCC1>[O:19]=[C:12]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:11][CH2:10][C:7]1[CH:8]=[CH:9][C:4]([C:3]([OH:20])=[O:2])=[CH:5][CH:6]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 18618679HCID 18618679, Verbindung

Produkt 1

HCID 22251491HCID 22251491, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21881883Oxolane--water (1/1)Lösungsmittel

Versuchsvorschrift

To a solution of methyl ester 47 (195 mg, 0.73 mmol) in water/THF (1:1, 0.07M) was added LiOH (46 mg, 1.1 mmol). The resulting solution was stirred overnight at room temperature or until no starting material was detected by TLC. HCl 1N was added and the solution was extracted with EtOAc and the organic layer was dried over anhydrous MgSO4. Filtration and evaporation of the solvent under vacuum followed by purification by column chromatography using 10% MeOH/CH2Cl2, gave the title compound.

Aufarbeitung

  1. extractionthe solution was extracted with EtOAc
  2. dry with materialthe organic layer was dried over anhydrous MgSO4
  3. filtrationFiltration and evaporation of the solvent under vacuum
  4. customfollowed by purification by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-3f394f95063044c79989c7f2239ecea6
Quelldatensatz
uspto-grants-2003_04
Patentnummer
US06541661B1

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