m-Chloroperbenzoic acid → HCID 23018243, 화합물

HRID 1348748노트

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HRID 1348748 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 23018243HCID 23018243, 화합물수율 44.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-21528cfaf4a844eca04e173f6d62ebeb
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211577B2

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