1,3-Dimethyluracil → HCID 178516350、化合物

HRID 538973ノート

反応式

HRID 538973 の反応式
[Na].[NH:2]1[CH:6]=[CH:5][C:4]([NH2:7])=[N:3]1.CN1[CH:14]=[CH:13][C:12](=[O:15])N(C)C1=O>CCO>[N:2]1[N:3]2[CH:14]=[CH:13][C:12]([OH:15])=[N:7][C:4]2=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 701221,3-DimethyluracilHCID 5360545SodiumHCID 178418806HCID 178418806、化合物

生成物 1

HCID 178516350HCID 178516350、化合物収率 53%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of dry EtOH (500 mL) was added sodium (22.1 g, 481 mmol) under a cold water bath. After complete dissolution, 1H-pyrazol-3-amine (40.0 g, 481 mmol) and 1,3-dimethylpyrimidine-2,4(1H,3H)-dione (101 g, 722 mmol) were added. The reaction mixture was heated at reflux for 4 hours. After cooling, the white solid was collected by filtration, washed with cold EtOH and dried under vacuum. The crude solid was suspended in minimum amount of water and the pH of the solution was adjusted to 5 by dropwise addition of acetic acid. The precipitated solid was collected by filtration, re-dissolved in MeOH and concentrated by rotary evaporation to azeotrope any remaining water to afford pyrazolo[1,5-a]pyrimidin-5-ol (34.3 g, 53%).

後処理

  1. additionwere added
  2. temperatureThe reaction mixture was heated
  3. temperatureat reflux for 4 hours
  4. temperatureAfter cooling
  5. filtrationthe white solid was collected by filtration
  6. washwashed with cold EtOH
  7. customdried under vacuum
  8. additionthe pH of the solution was adjusted to 5 by dropwise addition of acetic acid
  9. filtrationThe precipitated solid was collected by filtration
  10. dissolutionre-dissolved in MeOH
  11. concentrationconcentrated by rotary evaporation

出典と根拠

ORDレコード
ord-d904bb8008774dc29cdc37cc7eb1cf94
出典データセット
uspto-grants-2014_10
特許番号
US08865726B2

反応ノート

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