Formic Acid → HCID 178479550、化合物

HRID 514683

反応式

HRID 514683 の反応式
[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
81 °C

実験手順

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.

後処理

  1. temperatureSubsequently, after cooling to 58° C.
  2. temperatureAfter cooling the mixture to 20° C.
  3. filtrationthe crystal was collected by filtration
  4. washwashed with 20 mL of acetone

出典と根拠

ORDレコード
ord-c57fb60b21d340dab784a965b37050d4
出典データセット
uspto-grants-2015_08
特許番号
US09108928B2

関連ノート

読み込み中…