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

HRID 394480

反応式

HRID 394480 の反応式
[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

参加物

7

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 26052Sodium tungstate触媒

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-bd9f0d4d6bbb4dd4b3bc580128c3cb66
出典データセット
uspto-grants-2003_08
特許番号
US06602872B1

関連ノート

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