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Hydrochloric Acid → Ethyl 2-hydroxy-3-nitrobenzoate

HRID 912423
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HRID 912423 반응식
[OH:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl.[CH2:15](O)[CH3:16]>>[CH2:15]([O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:2]=1[OH:1])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 68073-Nitrosalicylic acid

생성물 1

HCID 12157235Ethyl 2-hydroxy-3-nitrobenzoate수율 86%

실험 절차

To a solution of 2-hydroxy-3-nitrobenzoic acid 10.0 g (55 mmol) in ethanol 100 mL was added dropwise 2 mL of conc. HCl, followed by stirring for 24 hrs under reflex. The mixture was cooled to room temperature, concentrated in a vacuum, and diluted with ethyl acetate. This dilution was washed with an aqueous saturated sodium bicarbonate solution and an aqueous saturated NaCl solution, dried over magnesium sulfate and concentrated in a vacuum. The concentrate was purified using column chromatography (developing solvent: ethylacetate/hexane=1/4) to afford the title compound 10.0 g (yield 86%).

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  • concentrationconcentrated in a vacuum
  • additiondiluted with ethyl acetate
  • washThis dilution was washed with an aqueous saturated sodium bicarbonate solution
  • dry with materialan aqueous saturated NaCl solution, dried over magnesium sulfate
  • concentrationconcentrated in a vacuum
  • customThe concentrate was purified
  • 출처 및 근거

    ORD 기록
    ord-a2383fa2da67456ab7326ffbfd54569c
    출처 데이터셋
    uspto-grants-2011_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08026235B1

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