Phosphorus oxychloride → 6-Chloro-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione

HRID 648888ノート

反応式

HRID 648888 の反応式
[CH3:1][N:2]1[C:9](=O)[CH2:8][C:6](=[O:7])[N:5]([CH3:11])[C:3]1=[O:4].P(Cl)(Cl)([Cl:14])=O>O>[Cl:14][C:9]1[N:2]([CH3:1])[C:3](=[O:4])[N:5]([CH3:11])[C:6](=[O:7])[CH:8]=1

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 69860Dimethylbarbituric acid

生成物 1

HCID 814426-Chloro-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 110 g of the 1,3-dimethylbarbituric acid was added 32 ml of water, and 800 ml of phosphorus oxychloride was added dropwise thereto. After heating at reflux for 1.5 hours, the phosphorus oxychloride was distilled away under normal pressure, and the residue, while hot, was poured onto ice. The precipitated crystals were collected by filtration. The filtrate was extracted three times with chloroform and dried over anhydrous sodium sulfate. The chloroform was then removed by distillation, and the resulting residue was combined with the aforesaid crystals. Recrystallization from water gave 80 g of 6-chloro-1,3-dimethyluracil.

後処理

  1. additionwas added dropwise
  2. temperatureAfter heating
  3. temperatureat reflux for 1.5 hours
  4. distillationthe phosphorus oxychloride was distilled away under normal pressure
  5. additionthe residue, while hot, was poured onto ice
  6. filtrationThe precipitated crystals were collected by filtration
  7. extractionThe filtrate was extracted three times with chloroform
  8. dry with materialdried over anhydrous sodium sulfate
  9. customThe chloroform was then removed by distillation
  10. customRecrystallization from water

出典と根拠

ORDレコード
ord-2188cdefb9dd4f449ba9968f6d9127fa
出典データセット
uspto-grants-1988_04
特許番号
US04737442

反応ノート

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