Hydrochloric Acid → HCID 178479550, compound
Reaction equation
[NH2:1][CH:2]([C:6]([NH2:8])=[O:7])[C:3]([NH2:5])=[O:4].O.[C:10]1(C)C=CC(S(O)(=O)=[O:17])=CC=1.C(OCC)(OCC)OCC.[ClH:31]>O.CC(O)C>[OH2:4].[OH2:17].[ClH:31].[OH:4][C:3]1[NH:5][CH:10]=[N:1][C:2]=1[C:6]([NH2:8])=[O:7]Participants
Conditions
- Temperature
- 82 °C
Procedure
Under the nitrogen atmosphere, 10.0 g of 2-aminomalonamide and 81.2 mg of p-toluene sulfonic acid monohydrate were added to 200 mL of 2-propanol. After heating to 82° C., 35.4 mL of triethyl orthoformate was added dropwise to the mixture over 5 minutes. Subsequently, the reaction mixture was stirred for 3 hours at 80° C. Color of the reaction liquid was deep blue when the reaction was completed. Subsequently, after cooling to 57° C., the reaction mixture was added with 10 mL of water followed by 8 mL of conc. hydrochloric acid. After cooling the reaction mixture to 5° C., the crystal was collected by filtration and then washed with 40 mL of acetone to give 15.6 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate as a green crystal.
Workup
- customColor of the reaction liquid
- temperatureSubsequently, after cooling to 57° C.
- temperatureAfter cooling the reaction mixture to 5° C.
- filtrationthe crystal was collected by filtration
- washwashed with 40 mL of acetone
Sources & evidence
- ORD record
- ord-1175c732b4f64a8287d11436880a3c5a
- Source dataset
- uspto-grants-2015_08
- Patent number
- US09108928B2
Reaction notes
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