6-Methyluracil → HCID 178429729、化合物

HRID 477553

反応式

HRID 477553 の反応式
[CH3:1][C:2]1[NH:7][C:6](=[O:8])[NH:5][C:4](=O)[CH:3]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:11]>N1C=CC=CC=1>[OH:8][C:6]1[N:5]=[C:4]([SH:11])[CH:3]=[C:2]([CH3:1])[N:7]=1

参加物

4

反応物 2

HCID 122836-MethyluracilHCID 14817Phosphorus sulfide (P2S5)

生成物 1

HCID 178429729HCID 178429729、化合物収率 136.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
50 °C

実験手順

6-Methyluracil (25.0 g) was suspended in 1 liter of distilled pyridine with stirring and heated at 50° C. into solution. Phosphorus pentasulfide (12.6 g) was then added, and the mixture was refluxed for 20 hours. The solution was concentrated under reduced pressure, then the residue was refluxed with 500 ml of ethanol for one hour. Insoluble materials were removed by filtration and the filtrate was concentrated under reduced pressure. The residue was recrystallized from ethanol, affording 5.5 g of the objective compound as colorless crystals.

後処理

  1. temperaturethe mixture was refluxed for 20 hours
  2. concentrationThe solution was concentrated under reduced pressure
  3. temperaturethe residue was refluxed with 500 ml of ethanol for one hour
  4. customInsoluble materials were removed by filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-8803435dd1da4637b5700b006de1fda9
出典データセット
uspto-grants-1989_12
特許番号
US04888332

関連ノート

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