Pyridoxine Hydrochloride → Pyridoxine

HRID 1972117

Reaktionsgleichung

Reaktionsgleichung von HRID 1972117
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([CH2:10][OH:11])[C:3]=1[OH:12].Cl>O>[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([CH2:10][OH:11])[C:3]=1[OH:12]

Komponenten

3

Edukt 1

HCID 6019Pyridoxine Hydrochloride

Produkt 1

HCID 1054Pyridoxine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

In a second alternative and preferred workup, the reaction mixture (following complete conversion to compound (C)) is cooled to 20° C. and diluted with water (approximately 2.80 L of water for every 1 kg of starting pyridoxine HCl). After phase separation the organic phase is washed with water. The combined aqueous phases are reextracted twice with TBME. The combined TBME phases are washed once with saturated NaHCO3-solution and once with diluted brine. The MTBE-product solution is concentrated to a concentration of about 50% and stored at room temperature until it is further converted. If this second alternative workup is used, the volume of MTBE in the synthetic step is preferably reduced by about 26%.

Aufarbeitung

  1. customAfter phase separation the organic phase
  2. washis washed with water
  3. washThe combined TBME phases are washed once with saturated NaHCO3-solution and once with diluted brine
  4. concentrationThe MTBE-product solution is concentrated to a concentration of about 50%
  5. customstored at room temperature until it

Quellen und Nachweise

ORD-Eintrag
ord-cc4bff35dda74e18b4029cc32dff8e2f
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08431712B2

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