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Disodium disulfite → 6-[[1-Phenyl-2-propanesulfinyl-1H-benzimidazol-6-yl]oxy]Hexanoic Acid Methyl Ester

HRID 1070847
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HRID 1070847 반응식
[CH3:1][O:2][C:3](=[O:29])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:11]=[CH:12][C:13]2[N:17]=[C:16]([S:18][CH2:19][CH2:20][CH3:21])[N:15]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:14]=2[CH:28]=1.ClC1C=CC=C(C(OO)=[O:38])C=1.S(OS([O-])=O)([O-])=O.[Na+].[Na+]>ClCCl>[CH3:1][O:2][C:3](=[O:29])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:11]=[CH:12][C:13]2[N:17]=[C:16]([S:18]([CH2:19][CH2:20][CH3:21])=[O:38])[N:15]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:14]=2[CH:28]=1
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참가 물질

5

반응물 3

HCID 24346Disodium disulfiteHCID 70297m-Chloroperbenzoic acidHCID 102234206-[[1-phenyl-2-propylmercapto-1H-benzimidazol-6-yl]oxy]hexanoic acid methyl ester

생성물 1

HCID 101596616-[[1-Phenyl-2-propanesulfinyl-1H-benzimidazol-6-yl]oxy]Hexanoic Acid Methyl Ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
20 °C

실험 절차

80 mg of 6-[[1-phenyl-2-propylmercapto-1H-benzimidazol-6-yl]oxy]hexanoic acid methyl ester was dissolved in 2 ml of dichloromethane, mixed with 56 mg of m-chloroperbenzoic acid (about 60%), and the mixture was stirred for 10 minutes at 20° C. It was mixed with sodium disulfite solution, extracted twice with dichloromethane, the combined organic phases were washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution, dried on sodium sulfate and concentrated by evaporation in a vacuum. The residue was purified by column chromatography on silica gel. 30 mg was obtained.

후처리

  1. extractionextracted twice with dichloromethane
  2. washthe combined organic phases were washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution
  3. customdried on sodium sulfate
  4. concentrationconcentrated by evaporation in a vacuum
  5. customThe residue was purified by column chromatography on silica gel
  6. custom30 mg was obtained

출처 및 근거

ORD 기록
ord-c366972d6a134d48912987c2f1b6fdd4
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06903126B2

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