Acetic Anhydride → 6-Amino-1-ethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

HRID 1758917

反応式

HRID 1758917 の反応式
[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

反応物 3

HCID 7918Acetic AnhydrideHCID 9740Cyanoacetic acidHCID 12254Ethylurea

生成物 1

HCID 8538996-Amino-1-ethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

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

  1. temperatureAfter cooling
  2. filtrationwhite crystals were filtered off
  3. washwashed with ethanol
  4. stirringThis was stirred in 1 liter of hot water
  5. addition160 ml of 2 N NaOH was added in portions so the solution the whole time
  6. temperatureThe reaction mixture was refluxed for 20 minutes
  7. temperatureAfter cooling
  8. 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

関連ノート

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