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Ethanol → HCID 58424985, 화합물

HRID 2409446
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HRID 2409446 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:12]([O-:14])=[O:13])[CH:11]=1)[C:6]([OH:8])=[O:7].S(Cl)(Cl)=O.[CH2:19](O)[CH3:20]>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:12]([O-:14])=[O:13])[CH:11]=1)[C:6]([O:8][CH2:19][CH3:20])=[O:7]
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참가 물질

4

반응물 3

HCID 702EthanolHCID 24386Thionyl ChlorideHCID 53002123-Methoxy-5-nitrobenzoic acid

생성물 1

HCID 58424985HCID 58424985, 화합물수율 85.6%

실험 절차

The compound (5.33 g, 27.0 mmol) prepared in step 1 was dissolved in absolute ethanol (55.0 ml), added dropwise with thionyl chloride (2.96 ml, 40.55 mmol) at 0° C. The resulting mixture was refluxed for 6 hours. After completion, the reaction mixture was concentrated under reduced pressure and mixed with sodium bicarbonate aqueous solution. The mixture was extracted with dichloromethan, dried over anhydrous magnesium sulfate, and concentrated to dryness. The residue was then purified by flash column chromatography (dichloromethane:hexane=4:1) to obtain the title compound (5.1 g, yield: 85.6%, ivory solid).

후처리

  1. temperatureThe resulting mixture was refluxed for 6 hours
  2. concentrationAfter completion, the reaction mixture was concentrated under reduced pressure
  3. additionmixed with sodium bicarbonate aqueous solution
  4. extractionThe mixture was extracted with dichloromethan
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated to dryness
  7. customThe residue was then purified by flash column chromatography (dichloromethane:hexane=4:1)

출처 및 근거

ORD 기록
ord-58939c9f7446408ab52f1b6405e7cb91
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815891B2

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