Reaktionsgleichung
[NH2:1][CH:2]([C:6]([NH2:8])=[O:7])[C:3]([NH2:5])=[O:4].[CH:9](O)=[O:10].C(OCC)(OCC)OCC.[ClH:22]>O.CC(O)C>[OH2:4].[OH2:10].[ClH:22].[OH:4][C:3]1[NH:5][CH:9]=[N:1][C:2]=1[C:6]([NH2:8])=[O:7]Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 81 °C
Versuchsvorschrift
Under the nitrogen atmosphere, 5.00 g of 2-aminomalonamide and 20 mg of formic acid were added to 80 mL of 2-propanol. After heating to 81° C., 17.7 mL of triethyl orthoformate was added to the mixture over 14 minutes. Subsequently, the reaction mixture was stirred for 6 hours and 33 minutes at 83° C. Subsequently, after cooling to 58° C., the reaction mixture was added dropwise with 5 mL of water followed by 4 mL of conc. hydrochloric acid. After cooling the mixture to 20° C., the crystal was collected by filtration and then washed with 20 mL of acetone to give 8.05 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate as a yellow crystal.
Aufarbeitung
- temperatureSubsequently, after cooling to 58° C.
- temperatureAfter cooling the mixture to 20° C.
- filtrationthe crystal was collected by filtration
- washwashed with 20 mL of acetone
Quellen und Nachweise
- ORD-Eintrag
- ord-c57fb60b21d340dab784a965b37050d4
- Quelldatensatz
- uspto-grants-2015_08
- Patentnummer
- US09108928B2
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