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Hydrogen Peroxide → 5-(2-Methylsulfonylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-4,5-dihydro-2H-pyridazin-3-one

HRID 394475
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인쇄 미리보기

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HRID 394475 반응식
CS[C:3]1[N:8]=[C:7]([CH:9]2[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=3)=[N:13][NH:12][C:11](=[O:25])[CH2:10]2)[CH:6]=[CH:5][N:4]=1.OO.[CH3:28]O.[S:30](S([O-])=O)([O-:32])=[O:31].[Na+].[Na+]>[O-][W]([O-])(=O)=O.[Na+].[Na+].C(OCC)(=O)C>[CH3:28][S:30]([C:3]1[N:8]=[C:7]([CH:9]2[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=3)=[N:13][NH:12][C:11](=[O:25])[CH2:10]2)[CH:6]=[CH:5][N:4]=1)(=[O:32])=[O:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 784Hydrogen PeroxideHCID 887MethanolHCID 24489Sodium DithioniteHCID 181766265-(2-Methylsulfanylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-4,5-dihydro-2H-pyridazin-3-one

생성물 1

HCID 181766135-(2-Methylsulfonylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-4,5-dihydro-2H-pyridazin-3-one

시약·촉매·용매 2

HCID 26052
Sodium tungstate
촉매
HCID 8857Ethyl Acetate용매

실험 절차

Compound 6 (17.8 mmol), sodium tungstate (587 mg, 1.78 mmol), 30% hydrogen peroxide (8.07 mL, 71.2 mmol), methanol (20 mL), and ethyl acetate (200 mL) were combined under argon, then heated to reflux for 4 h. The solution was cooled and aqueous sodium hydrosulfite was added. The methanol was removed in vacuo and saturated sodium bicarbonate was added. The resulting suspension was extracted several times with methylene chloride. The combined organic extracts were washed successively with water and brine. The organic layer was dried with anhydrous sodium sulfate then concentrated in vacuo to give Compound 7 as a foam: 5.0 g (13 mmol, 73% (two steps))

후처리

  1. temperatureheated
  2. temperatureto reflux for 4 h
  3. temperatureThe solution was cooled
  4. customThe methanol was removed in vacuo and saturated sodium bicarbonate
  5. additionwas added
  6. extractionThe resulting suspension was extracted several times with methylene chloride
  7. washThe combined organic extracts were washed successively with water and brine
  8. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  9. concentrationthen concentrated in vacuo

출처 및 근거

ORD 기록
ord-c0547385b9c942c6ba5de8f00893f129
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06602872B1

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