Hydrogen Peroxide → HCID 178431782、化合物

HRID 241002ノート

反応式

HRID 241002 の反応式
OO.[CH:3]([C:6]1[NH:11][C:10](=S)[NH:9][C:8](=[O:13])[C:7]=1[CH3:14])([CH3:5])[CH3:4].C(=O)([O-])[O-].[Na+].[Na+].S([O-])([O-])(=O)=S.[Na+].[Na+]>O>[CH:3]([C:6]1[N:11]=[CH:10][N:9]=[C:8]([OH:13])[C:7]=1[CH3:14])([CH3:5])[CH3:4]

参加物

6

反応物 4

HCID 784Hydrogen PeroxideHCID 10340Sodium CarbonateHCID 24477Sodium ThiosulfateHCID 12512044HCID 12512044、化合物

生成物 1

HCID 178431782HCID 178431782、化合物収率 30.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

To a solution of 30% hydrogen peroxide (12 mL) and water (23 mL) was slowly added 6-isopropyl-5-methyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (1.0 g, 5.4 mmol). The reaction mixture was stirred at 70° C. for 3 h. After cooling to room temperature, saturated sodium carbonate was slowly added until the pH reached 10. To this mixture was slowly added a 1 M solution of sodium thiosulfate until residual peroxide was quenched, whereupon the aqueous solution was concentrated to dryness. The residue was suspended in chloroform (100 mL), filtered to remove inorganic salts and the filtrate concentrated to provide 6-isopropyl-5-methylpyrimidin-4-ol (0.25 g, 30% yield) as a white solid that was used without further purification. MS (EI) for C8H12N2O: 153 (MH+).

後処理

  1. temperatureAfter cooling to room temperature
  2. customwas quenched, whereupon the aqueous solution
  3. concentrationwas concentrated to dryness
  4. filtrationfiltered
  5. customto remove inorganic salts
  6. concentrationthe filtrate concentrated

出典と根拠

ORDレコード
ord-0ca1d605bdbf4a15acb0c366a0bc203b
出典データセット
uspto-grants-2014_02
特許番号
US08648066B2

反応ノート

読み込み中…