Water → Lipoic acid

HRID 2215861Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2215861
[CH2:1]([CH2:7][C@@H:8]([SH:12])[CH2:9][CH2:10][SH:11])[CH2:2][CH2:3][C:4]([OH:6])=[O:5].O.[OH-].[Na+].OS(O)(=O)=O>C1(C)C=CC=CC=1>[CH2:9]1[C@@H:8]([CH2:7][CH2:1][CH2:2][CH2:3][C:4]([OH:6])=[O:5])[S:12][S:11][CH2:10]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 9834298(R)-Dihydrolipoic acid

Produkt 1

HCID 6112Lipoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

125.5 g of the dihydrolipoic acid solution are stirred in 5 l of completely deionized water in a 10 l round-bottomed flask, and the solution is adjusted to pH 8.5 using dilute sodium hydroxide solution and treated with catalytic amounts of Fe(III) sulfate solution. Air is introduced until the color lightens. After addition of 600 ml of toluene, the mixture is adjusted to pH 2 using H2SO4. The phases are separated and the water phase is extracted once with toluene. The combined toluene phases are concentrated to about 25% of the volume. The residue is treated with 600 ml of heptane, stirred under nitrogen and then forced through a filter loaded with silica gel. The filter is washed with toluene/heptane mixture.

Aufarbeitung

  1. additionAir is introduced until the color lightens
  2. customThe phases are separated
  3. extractionthe water phase is extracted once with toluene
  4. concentrationThe combined toluene phases are concentrated to about 25% of the volume
  5. additionThe residue is treated with 600 ml of heptane
  6. washThe filter is washed with toluene/heptane mixture

Quellen und Nachweise

ORD-Eintrag
ord-62d0bdb214414b959920add42917bbc3
Quelldatensatz
uspto-grants-2006_09
Patentnummer
US07109362B2

Notizen zur Reaktion

Wird geladen…