Water → 6-chloro-3-methylpyrimidine-2,4(1H,3H)-dione

HRID 377609ノート

反応式

HRID 377609 の反応式
[CH3:1][N:2]1[C:9](=[O:10])[CH2:8][C:6](=O)[NH:5][C:3]1=[O:4].O.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:6]1[NH:5][C:3](=[O:4])[N:2]([CH3:1])[C:9](=[O:10])[CH:8]=1

参加物

4

反応物 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 757221-Methyl-2,4,6(1H,3H,5H)-pyrimidinetrione

生成物 1

HCID 961416-chloro-3-methylpyrimidine-2,4(1H,3H)-dione

実験手順

1-Methylbarbituric acid (10 g) was suspended in phosphorus oxychloride (70 ml). Water (2 ml) was added and the mixture was heated at reflux for 40 minutes. The reaction was allowed to cool and was then concentrated under reduced pressure. The residue was poured onto a mixture of ice and water (200 ml). When the ice had melted, the precipitated solid was collected, washed with water and dried in vacuo at 50° C. to give the sub-title compound (6.86 g) as a yellow solid.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 40 minutes
  3. temperatureto cool
  4. concentrationwas then concentrated under reduced pressure
  5. additionThe residue was poured onto a mixture of ice and water (200 ml)
  6. customthe precipitated solid was collected
  7. washwashed with water
  8. customdried in vacuo at 50° C.

出典と根拠

ORDレコード
ord-4b900d2df6f8472bb0082e6245023774
出典データセット
uspto-grants-2000_02
特許番号
US06028074

反応ノート

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