反応式
[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]参加物
7
反応条件
- 温度
- 80 °C
実験手順
Under the nitrogen atmosphere, 10 g of 2-aminomalonamide and 19.7 mg of formic acid were added to 200 mL of 2-propanol. After heating to 80° C., 35.4 mL of triethyl orthoformate was added dropwise to the mixture over 5 minutes. Subsequently, the reaction mixture was stirred for 8 hours at 80° C. Color of the reaction liquid was pale blue when the reaction was completed. Subsequently, after cooling to 56° C., the reaction mixture was added with 10 mL of water followed by 8 mL of conc. hydrochloric acid. After cooling with water, the crystal was collected by filtration and then washed with 40 mL of acetone to give 16 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate as a pale yellowish green crystal.
後処理
- customColor of the reaction liquid
- temperatureSubsequently, after cooling to 56° C.
- filtrationthe crystal was collected by filtration
- washwashed with 40 mL of acetone
出典と根拠
- ORDレコード
- ord-1b69dabac6524e80a14330ee27d18147
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09108928B2
関連ノート
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