m-Chloroperbenzoic acid → HCID 23018243、化合物

HRID 1348748ノート

反応式

HRID 1348748 の反応式
[CH:1]1([CH2:4][N:5]2[C:10](=[O:11])[C:9]([CH2:12][O:13][S:14]([CH3:17])(=[O:16])=[O:15])=[CH:8][C:7]([C:18]3[CH:23]=[CH:22][C:21]([S:24][CH3:25])=[CH:20][CH:19]=3)=[N:6]2)[CH2:3][CH2:2]1.ClC1C=CC=C(C(OO)=[O:34])C=1.S([O-])(O)=O.[Na+]>C(Cl)Cl>[CH:1]1([CH2:4][N:5]2[C:10](=[O:11])[C:9]([CH2:12][O:13][S:14]([CH3:17])(=[O:16])=[O:15])=[CH:8][C:7]([C:18]3[CH:23]=[CH:22][C:21]([S:24]([CH3:25])=[O:34])=[CH:20][CH:19]=3)=[N:6]2)[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 70297m-Chloroperbenzoic acidHCID 219915572-cyclopropylmethyl-4-methanesulfonyloxymethyl-6-[4-(methyl thio)phenyl]-2H-pyridazin-3-oneHCID 23665763Sodium Bisulfite

生成物 1

HCID 23018243HCID 23018243、化合物収率 44.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2-cyclopropylmethyl-4-methanesulfonyloxymethyl-6-[4-(methylthio)phenyl]-2H-pyridazin-3-one (300 mg, 0.79 mmol) in methylene chloride (10 mL) was added dropwise at −20° C. a solution of 3-chloroperbenzoic acid (204 mg, 1.12 mmol) in methylene chloride (2 mL), and at the same temperature, the mixture was stirred for 30 minutes. A 10% aqueous sodium hydrogensulfite was added to the reaction mixture, and then, the mixture was extracted with chloroform. The extract was successively washed with a saturated aqueous sodium hydrogencarbonate and brine, and was then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue was recrystallized from chloroform-hexane to yield the title compound as a colorless crystalline powder (139 mg, 44.5%).

後処理

  1. extractionthe mixture was extracted with chloroform
  2. washThe extract was successively washed with a saturated aqueous sodium hydrogencarbonate and brine
  3. dry with materialwas then dried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customThe residue was recrystallized from chloroform-hexane

出典と根拠

ORDレコード
ord-21528cfaf4a844eca04e173f6d62ebeb
出典データセット
uspto-grants-2007_05
特許番号
US07211577B2

反応ノート

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