Methanol → Methyl 2-((phenylcarbonothioyl)thio)acetate
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
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
- temperatureThe reaction mixture was refluxed for 4 hours
- concentrationThe reaction mixture was concentrated in vacuo and ethyl acetate
- additionwas added
- washThe mixture was washed with sat. aq. NaHCO3 and brine
- dry with materialdried over Na2SO4
- 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
反応ノート
読み込み中…