Hydrochloric Acid → HCID 178479550, compound
Reaction equation
[NH2:1][CH:2]([C:6]([NH2:8])=[O:7])[C:3]([NH2:5])=[O:4].[CH3:9]C([OH:12])C.C(OCC)(OCC)OCC.[ClH:23]>O>[OH2:4].[OH2:12].[ClH:23].[OH:4][C:3]1[NH:5][CH:9]=[N:1][C:2]=1[C:6]([NH2:8])=[O:7]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 80 °C
Procedure
Under the nitrogen atmosphere, 5.00 g of 2-aminomalonamide was added to 100 mL of 2-propanol. After heating to 80° C., 17.7 mL of triethyl orthoformate was added dropwise to the mixture over 30 minutes. Subsequently, the reaction mixture was stirred for 7 hours and 50 minutes at 83 to 84° C. Subsequently, after cooling to 50 to 60° C., the reaction mixture was added with an aqueous solution prepared with 4 mL of conc. hydrochloric acid and 5 mL of water. After cooling the mixture to 20 to 30° C., the crystal was collected by filtration and then washed with 25 mL of acetone to give 8.04 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate as a pale yellow crystal.
Workup
- temperatureSubsequently, after cooling to 50 to 60° C.
- additionthe reaction mixture was added with an aqueous solution
- temperatureAfter cooling the mixture to 20 to 30° C.
- filtrationthe crystal was collected by filtration
- washwashed with 25 mL of acetone
Sources & evidence
- ORD record
- ord-d07e51d2086344d9b8e4098df29598c4
- Source dataset
- uspto-grants-2015_08
- Patent number
- US09108928B2
Reaction notes
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