反応 #487573

ord-10417475da6d40dbb7657d2781a3f4df

反応方程式

O=P(Cl)(Cl)Cl
phosphoryl chloride
CN(C)C=O
DMF
O=C1CC(=O)NC(=O)N1
barbituric acid
O=CC1C(=O)NC(=O)NC1=O
2,4,6-trioxohexahydropyrimidine-5-carbaldehyde

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooling
  2. 2
    温度The mixture is cooled
  3. 3
    その他the precipitate is separated off
  4. 4
    洗浄rinsed with water
  5. 5
    その他dried at 45°
  6. 6
    その他giving 2.5 g of “1”

実験手順

9.03 ml of phosphoryl chloride are added dropwise to 2 ml of dry DMF with ice-cooling. 1.5 g of barbituric acid are subsequently added, and the mixture is stirred at 100° for 4 h. The mixture is cooled, poured into ice-water, the precipitate is separated off, rinsed with water and dried at 45°, giving 2.5 g of “1”.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08741896B2uspto-grants-2014_06