Potassium cyanate → 2,3-Dihydro-2-oxo-4,N,N-trimethyl-1H-imidazole-5-carboxamide
反応式
[CH3:1][N:2]([CH3:11])[C:3](=[O:10])[C:4](=[N:8]O)[C:5](=O)[CH3:6].[H][H].[O-:14][C:15]#[N:16].[K+]>C(O)C.Cl.O>[O:14]=[C:15]1[NH:16][C:5]([CH3:6])=[C:4]([C:3]([N:2]([CH3:11])[CH3:1])=[O:10])[NH:8]1参加物
7
実験手順
A solution of 15.8 g (0.1 mol) of N,N-dimethyl-2-(hydroxyimino)-3-oxobutanamide in 400 ml of ethanol and 100 ml of 2N hydrochloric acid over 2 g of catalyst (5% palladium on charcoal) is hydrogenated in a Paar shaker until 1 molar equivalent of hydrogen is taken up (3-5 hours). The catalyst is removed by filtration. A solution of 16.2 g (0.2 mol) of potassium cyanate in 80 ml of water is added, the solution is refluxed for 1 hour and concentrated until the product crystallizes. Recrystallization from 50% aqueous ethanol gives the title compound, m.p. 244°-246° C. (dec).
後処理
- custom(3-5 hours)
- customThe catalyst is removed by filtration
- temperaturethe solution is refluxed for 1 hour
- concentrationconcentrated until the product
- customcrystallizes
- customRecrystallization from 50% aqueous ethanol
出典と根拠
- ORDレコード
- ord-ea34432a812544cba5f70cb2d8c99279
- 出典データセット
- uspto-grants-1991_03
- 特許番号
- US05002961
反応ノート
読み込み中…