Potassium Hydroxide → HCID 19904422, Verbindung

HRID 2372419Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2372419
[C:1]([C:6]1([C:13](OCC)=[O:14])[CH2:11][CH2:10][CH2:9][CH2:8][C:7]1=[O:12])(OCC)=[O:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[K+].P([O-])([O-])(O)=O.[K+].[K+].P([O-])(O)(O)=O.[K+]>CCOCC.O>[OH:14][CH2:13][C:6]1([CH2:1][OH:2])[CH2:11][CH2:10][CH2:9][CH2:8][CH:7]1[OH:12]

Komponenten

8

Edukt 5

HCID 14797Potassium HydroxideHCID 24450Potassium Phosphate, DibasicHCID 224023Diethyl 2-oxocyclohexane-1,1-dicarboxylateHCID 516951Monobasic potassium phosphateHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 19904422HCID 19904422, VerbindungAusbeute 60,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

A solution of 2,2-dicarbethoxycyclohexanone (3.0 g.) in dry ether (15 ml.) was added dropwise to a stirred suspension of lithium aluminium hydride (1.4 g.) in dry ether (50 ml.) at 0°, under nitrogen. The mixture was refluxed, with stirring, for six hours. Potassium hydroxide (6 g.) in water (100 ml) was added to the stirred mixture. Dipotassium hydrogen phosphate (4.2 g.) and potassium dihydrogen phosphate (3.3 g.) in water (50 ml.) was added. Ether was removed by passing a current of nitrogen through the mixture. The resultant slurry was acidified with glacial acetic acid and the solid was filtered off. The filtrate was evaporated in vacuo. The residue was extracted with acetone and the solution was evaporated in vacuo. 2,2Di-(hydroxymethyl)-cyclohexanol (1.2 g.) was obtained as a pale yellow oil.

Aufarbeitung

  1. temperatureThe mixture was refluxed
  2. customEther was removed
  3. filtrationthe solid was filtered off
  4. customThe filtrate was evaporated in vacuo
  5. extractionThe residue was extracted with acetone
  6. customthe solution was evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b58d505661ee43bc907e035160e47acb
Quelldatensatz
uspto-grants-1992_03
Patentnummer
US05098929

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