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

HRID 1039165

反応式

HRID 1039165 の反応式
[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

参加物

4

反応物 3

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

生成物 1

HCID 71356278Methyl 2-((phenylcarbonothioyl)thio)acetate収率 97%

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-688984c870574770a6a80db22151b732
出典データセット
uspto-grants-2013_10
特許番号
US08552039B2

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