Lithium Hydroxide → HCID 21017824, Verbindung

HRID 644939

Reaktionsgleichung

Reaktionsgleichung von HRID 644939
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][C@H:9]2[C:15]([O:17]C)=[O:16])=[CH:4][CH:3]=1.[OH-].[Li+].Cl.[Cl-].[Na+].O>O1CCCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C@@H:8]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][C@H:9]2[C:15]([OH:17])=[O:16])=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 3939Lithium HydroxideHCID 68520286HCID 68520286, VerbindungHCID 131718760Hydrochloric acid brine

Produkt 1

HCID 21017824HCID 21017824, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A stirred mixture of 0.435 g (1.63 mmol) of methyl trans-2-(4-chlorophenyl)-5-oxocyclohexanecarboxylate (described in Step B of Example 1) and 1 N lithium hydroxide (3.26 mL, 3.26 mmol) in tetrahydrofuran (3.3 mL) was heated at reflux for approximately 1 h. After cooling to room temperature, the reaction mixture was poured into 1 N hydrochloric acid/brine (1:1) and extracted three times with methylene chloride. The combined organic extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. The residual crude title compound was used without further purification in the subsequent reaction.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for approximately 1 h
  3. extractionextracted three times with methylene chloride
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe residual crude title compound was used without further purification in the subsequent reaction

Quellen und Nachweise

ORD-Eintrag
ord-1efd9cc470724fba99bfaf4fda84b551
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07700778B2

Verknüpfte Notizen

Wird geladen…