Hydrogen Peroxide → HCID 178431782, 화합물

HRID 241002노트

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HRID 241002 반응식
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]

참가 물질

6

반응물 4

HCID 784Hydrogen PeroxideHCID 10340Sodium CarbonateHCID 24477Sodium ThiosulfateHCID 12512044HCID 12512044, 화합물

생성물 1

HCID 178431782HCID 178431782, 화합물수율 30.4%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-0ca1d605bdbf4a15acb0c366a0bc203b
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648066B2

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