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

HRID 78725

反応式

HRID 78725 の反応式
[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

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 98%

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-d3aef15bfca74418ab7803638a34a11d
出典データセット
uspto-grants-2014_09
特許番号
US08841449B2

関連ノート

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