Lithium Hydroxide → HCID 18628853, Verbindung

HRID 1060732Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1060732
[CH:1]1([CH2:7][CH:8]([C:14]([O:16]CC)=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[OH-].[Li+]>C(O)C.O>[CH:1]1([CH2:7][CH:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:14]([OH:16])=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Komponenten

5

Edukt 2

HCID 3939Lithium HydroxideHCID 599487Diethyl 2-cyclohexylmethylmalonate

Produkt 1

HCID 18628853HCID 18628853, VerbindungAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

A solution comprised of diethyl 2-cyclohexylmethylmalonate (12.817 g, 50 mmol) in ethanol (100 mL) was treated with a solution of comprised of lithium hydroxide (1.198 g, 50 mmol) in water (50 mL) and the mixture was stirred for approximately 12 hours at ambient temperature. Solvent was removed by evaporation and the residue was diluted with water (50 mL). The dilution was extracted with diethyl ether (2×). The aqueous layer was cooled to 0° C., acidified to pH 1.5 with 1N hydrochloric acid (50 mL), saturated with solid sodium chloride and then extracted with ethyl acetate (2×). The combined ethyl acetate extracts were dried (MgSO4) and concentrated. The residue was dried to provide 3-cyclohexyl-2-ethoxycarbonylpropionic acid (8.52 g, 37 mmol) as an oil.

Aufarbeitung

  1. additionwas treated with a solution
  2. customSolvent was removed by evaporation
  3. additionthe residue was diluted with water (50 mL)
  4. extractionThe dilution was extracted with diethyl ether (2×)
  5. temperatureThe aqueous layer was cooled to 0° C.
  6. extractionextracted with ethyl acetate (2×)
  7. dry with materialThe combined ethyl acetate extracts were dried (MgSO4)
  8. concentrationconcentrated
  9. customThe residue was dried

Quellen und Nachweise

ORD-Eintrag
ord-becbf32b2d8c4bc9abc5bc8a5b2471ba
Quelldatensatz
uspto-grants-2003_02
Patentnummer
US06525036B2

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