Reaktionsgleichung
O.O.Cl.[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11].Cl.C([O-])=O.[Na+]>>[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11]Komponenten
4
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
Under the nitrogen atmosphere, 20.0 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate prepared according to the method of Reference Example 2 was added to 240 mL of 0.45 mol/L hydrochloric acid and dissolved therein by heating to 50° C. At 50° C., 40 mL aqueous solution containing 14.3 g of sodium formate was added dropwise thereto over 33 minutes. The reaction mixture was cooled. The crystal was collected by filtration and then washed with a mixture liquid containing 20 mL of acetone and 40 mL of water followed by 60 mL of acetone to give 12.8 g of 5-hydroxy-1H-imidazole-4-carboxamide.3/4 hydrate as a pale yellow crystal. The infrared absorption spectrum (ATR method) corresponds to that of Example 4.
Aufarbeitung
- dissolutiondissolved
- additionwas added dropwise
- temperatureThe reaction mixture was cooled
- filtrationThe crystal was collected by filtration
- washwashed with a mixture liquid
- additioncontaining 20 mL of acetone and 40 mL of water
Quellen und Nachweise
- ORD-Eintrag
- ord-46b3f5b3dd64454bb4070a247dba9925
- Quelldatensatz
- uspto-grants-2015_08
- Patentnummer
- US09108928B2
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