Hydrogen Peroxide → Dimethyl-[5-(2-methylsulfonylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-pyridazin-3-yl]amine

HRID 394480

반응식

HRID 394480 반응식
[CH3:1][N:2]([CH3:27])[C:3]1[N:4]=[N:5][C:6]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=2)=[C:7]([C:9]2[CH:14]=[CH:13][N:12]=[C:11]([S:15][CH3:16])[N:10]=2)[CH:8]=1.OO.CO.C(OCC)(=[O:34])C.[OH2:38]>[O-][W]([O-])(=O)=O.[Na+].[Na+]>[CH3:27][N:2]([CH3:1])[C:3]1[N:4]=[N:5][C:6]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=2)=[C:7]([C:9]2[CH:14]=[CH:13][N:12]=[C:11]([S:15]([CH3:16])(=[O:34])=[O:38])[N:10]=2)[CH:8]=1

참가 물질

7

반응물 5

HCID 784Hydrogen PeroxideHCID 887MethanolHCID 962WaterHCID 8857Ethyl AcetateHCID 18176616Dimethyl-[5-(2-methylsulfanylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-pyridazin-3-yl]amine

생성물 1

HCID 18176627Dimethyl-[5-(2-methylsulfonylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-pyridazin-3-yl]amine

시약·촉매·용매 1

HCID 26052Sodium tungstate촉매

실험 절차

Compound 71 (112 mg, 0.286 mmol), sodium tungstate (10 mg, 0.02 mmol), 30% hydrogen peroxide (130 μL, 1.14 mmol), methanol (2.0 mL), and ethyl acetate (20 mL) were combined under Argon and heated to reflux for 3d. The solution was cooled, poured into water and extracted several times with ethyl acetate. The combined organic extracts were dried with anhydrous sodium sulfate. Removal of the solvent in vacuo gave 72 as a solid: 109 mg (0.259 mmol, 91%)

후처리

  1. temperatureheated
  2. temperatureThe solution was cooled
  3. extractionextracted several times with ethyl acetate
  4. dry with materialThe combined organic extracts were dried with anhydrous sodium sulfate
  5. customRemoval of the solvent in vacuo

출처 및 근거

ORD 기록
ord-bd9f0d4d6bbb4dd4b3bc580128c3cb66
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06602872B1

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