Lithium hydroxide, monohydrate → HCID 19077644, Verbindung

HRID 1780826Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1780826
O[Li].O.[CH:4](=[C:6]1[CH2:10][CH:9]([C:11]([O:13]CC)=[O:12])[CH:8]([C:16]([O:18]CC)=[O:17])[CH2:7]1)[CH3:5]>O.C1COCC1>[CH:4](=[C:6]1[CH2:10][CH:9]([C:11]([OH:13])=[O:12])[CH:8]([C:16]([OH:18])=[O:17])[CH2:7]1)[CH3:5]

Komponenten

5

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 564797HCID 564797, Verbindung

Produkt 1

HCID 19077644HCID 19077644, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of LiOH.H2O (5.1 g, 120 mmol) in 130 ml of water is added dropwise at 0° C. to a solution of the compound from Example VIII (13.1 g, 54.5 mmol) in 70 ml of THF. The solution is stirred at room temperature for 20 h, the THF is stripped off in vacuo and the residue is extracted once with 40 ml of ether. The aqueous phase is brought to pH 2 with 10% strength hydrochloric acid and extracted three times with 200 ml of ethyl acetate each time. The combined ethyl acetate phases are dried over Na2SO4 and the solvent is stripped off in vacuo.

Aufarbeitung

  1. extractionthe residue is extracted once with 40 ml of ether
  2. extractionextracted three times with 200 ml of ethyl acetate each time
  3. dry with materialThe combined ethyl acetate phases are dried over Na2SO4

Quellen und Nachweise

ORD-Eintrag
ord-d5fa86465a0d4eb0a30caa40dc7443f1
Quelldatensatz
uspto-grants-1997_05
Patentnummer
US05631291

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