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m-Chloroperbenzoic acid → HCID 54274875, 화합물

HRID 1900184
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HRID 1900184 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([S:19][CH2:20][CH:21]([NH:23][C:24](=[O:36])[C@H:25]([CH:33]([CH3:35])[CH3:34])[NH:26][C:27]([O:29][CH:30]([CH3:32])[CH3:31])=[O:28])[CH3:22])=[CH:15][CH:14]=1>C(Cl)Cl>[F:12][C:13]1[CH:18]=[CH:17][C:16]([S:19]([CH2:20][CH:21]([NH:23][C:24](=[O:36])[C@H:25]([CH:33]([CH3:35])[CH3:34])[NH:26][C:27]([O:29][CH:30]([CH3:31])[CH3:32])=[O:28])[CH3:22])=[O:9])=[CH:15][CH:14]=1
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 53780799HCID 53780799, 화합물

생성물 1

HCID 54274875HCID 54274875, 화합물수율 69%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.3 g of m-chloroperbenzoic acid was added to a solution containing 2.5 g of N1 -[2-(4-fluorophenylthio)-1-methylethyl]-N2 -isopropoxycarbonyl-L-valinamide dissolved in 50 ml of methylene chloride, at 0° C. After the mixture was stirred for 5 hours at room temperature, the reaction mixture was filtered. The filtrate was washed successively with a saturated aqueous solution of potassium carbonate and water, the organic layer was dried over anhydrous sodium sulfate and the methylene chloride was removed under reduced pressure. The obtained residue was purified by column chromatography on silica gel, thus obtaining 1.8 g of the desired product in the form of a colorless prism-shaped crystal (yield: 69%).

후처리

  1. filtrationthe reaction mixture was filtered
  2. washThe filtrate was washed successively with a saturated aqueous solution of potassium carbonate and water
  3. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  4. customthe methylene chloride was removed under reduced pressure
  5. customThe obtained residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-94f328faf1bb4cb2a47113c58509d247
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05574064

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