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

HRID 78725

반응식

HRID 78725 반응식
[C:1]1([C:7]([S:9][CH2:10][C:11]([OH:13])=[O:12])=[S:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(Cl)(Cl)=O.[CH3:18]O>>[C:1]1([C:7]([S:9][CH2:10][C:11]([O:13][CH3:18])=[O:12])=[S:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 3

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

생성물 1

HCID 71356278Methyl 2-((phenylcarbonothioyl)thio)acetate수율 98%

실험 절차

2-((Phenylcarbonothioyl)thio)acetic acid (10 g, 47.1 mmol) was dissolved in 200 mL of methanol followed by the dropwise addition of thionylchloride (16 g, 120 mmol) at room temperature. The reaction mixture was refluxed for 4 hours. The reaction mixture was concentrated in vacuo and ethyl acetate was added. The mixture was washed with sat. aq. NaHCO3 and brine and dried over Na2SO4. The reaction mixture was concentrated in vacuo to afford Methyl 2-((phenylcarbonothioyl)thio)acetate 2 as brown oil (10.5 g, 98%).

후처리

  1. temperatureThe reaction mixture was refluxed for 4 hours
  2. concentrationThe reaction mixture was concentrated in vacuo and ethyl acetate
  3. additionwas added
  4. washThe mixture was washed with sat. aq. NaHCO3 and brine
  5. dry with materialdried over Na2SO4
  6. concentrationThe reaction mixture was concentrated in vacuo

출처 및 근거

ORD 기록
ord-d3aef15bfca74418ab7803638a34a11d
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841449B2

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