Acetic Anhydride → 6-Amino-1-ethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione
反応式
[C:1](CC(O)=O)#[N:2].[CH2:7]([NH:9][C:10]([NH2:12])=[O:11])[CH3:8].C(O[C:17](=[O:19])[CH3:18])(=O)C>>[NH2:2][C:1]1[N:9]([CH2:7][CH3:8])[C:10](=[O:11])[NH:12][C:17](=[O:19])[CH:18]=1参加物
4
実験手順
To a solution of 127.5 g (1.5 mol) cyanoacetic acid and 200 ml of acetic anhydride was added 120 g (1.36 mol) of ethylurea. The solution was stirred at 60°-70° C. for 2 hours. After cooling, white crystals were filtered off and washed with ethanol. Yield 153 g (74%) (I). This was stirred in 1 liter of hot water and 160 ml of 2 N NaOH was added in portions so the solution the whole time was basic. The reaction mixture was refluxed for 20 minutes and then neutralized with 5 N HCl. After cooling, white crystals were filtered off. Yield 100 g (65%) (II) NMR.
後処理
- temperatureAfter cooling
- filtrationwhite crystals were filtered off
- washwashed with ethanol
- stirringThis was stirred in 1 liter of hot water
- addition160 ml of 2 N NaOH was added in portions so the solution the whole time
- temperatureThe reaction mixture was refluxed for 20 minutes
- temperatureAfter cooling
- filtrationwhite crystals were filtered off
出典と根拠
- ORDレコード
- ord-03f980486b5944cdaf5d2a3bf9624134
- 出典データセット
- uspto-grants-1982_07
- 特許番号
- US04338319
反応ノート
読み込み中…