Sodium Acetate → HCID 178513824, Verbindung

HRID 514679

Reaktionsgleichung

Reaktionsgleichung von HRID 514679
O.O.Cl.[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11].C([O-])(=O)C.[Na+]>Cl>[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11]

Komponenten

4

Edukt 2

HCID 517045Sodium AcetateHCID 178479550HCID 178479550, Verbindung

Produkt 1

HCID 178513824HCID 178513824, VerbindungAusbeute 95,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

Under the nitrogen atmosphere, 10.0 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate prepared according to the method of Reference Example 2 was added to 120 mL of 0.45 mol/L hydrochloric acid and dissolved therein by heating to 40 to 50° C. At 50° C., 25 mL aqueous solution containing 10.3 g of sodium acetate was added dropwise thereto. pH of the reaction mixture was 4.0. After the dropwise addition was completed, the reaction solution was cooled to room temperature and stirred for 1 hour. The crystal was collected by filtration and then washed with a mixture liquid containing 10 mL of acetone and 20 mL of water followed by 30 mL of acetone to obtain 6.1 g of 5-hydroxy-1H-imidazole-4-carboxamide.3/4 hydrate as a gray crystal. The infrared absorption spectrum (ATR method) corresponds to that of Example 4.

Aufarbeitung

  1. dissolutiondissolved
  2. additionwas added dropwise
  3. additionAfter the dropwise addition
  4. temperaturethe reaction solution was cooled to room temperature
  5. filtrationThe crystal was collected by filtration
  6. washwashed with a mixture liquid
  7. additioncontaining 10 mL of acetone and 20 mL of water

Quellen und Nachweise

ORD-Eintrag
ord-45c8c3cf8d3348f38353dac2cdea7886
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09108928B2

Verknüpfte Notizen

Wird geladen…