Methanol → Methyl 2-((phenylcarbonothioyl)thio)acetate

HRID 1616551

반응식

HRID 1616551 반응식
[C:1]([S:9][CH2:10][C:11]([OH:13])=[O:12])(=[S:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)(Cl)=O.[CH3:18]O>>[CH3:18][O:12][C:11](=[O:13])[CH2:10][S:9][C:1](=[S:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 70336((Phenylthioxomethyl)thio)acetic acid

생성물 1

HCID 71356278Methyl 2-((phenylcarbonothioyl)thio)acetate수율 97%

실험 절차

Add a solution of thiobenzoylsulfanylacetic acid (5.5 g, 26.0 mmol) in methanol (100 mL) and to a solution of thionyl chloride (52 mL) at room temperature under nitrogen and heat the mixture at reflux for 12 hours. Remove the solvent under reduced pressure, dissolve the residue in ethyl acetate (200 mL), wash with saturated NaHCO3 (200 mL) and brine (200 mL) solutions, and dry over sodium sulfate. Remove the solvent under reduced pressure to provide thiobenzoylsulfanylacetic acid methyl ester (5.7 g, 97%).

후처리

  1. temperatureat reflux for 12 hours
  2. customRemove the solvent under reduced pressure
  3. dissolutiondissolve the residue in ethyl acetate (200 mL)
  4. washwash with saturated NaHCO3 (200 mL) and brine (200 mL) solutions
  5. dry with materialdry over sodium sulfate
  6. customRemove the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-44090259540147818b7e3f401aec688e
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765796B2

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