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Methanol → Methyl 2-((phenylcarbonothioyl)thio)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | ((Phenylthioxomethyl)thio)acetic acid | HCID 70336 | — |
| 生成物 | Methyl 2-((phenylcarbonothioyl)thio)acetate | HCID 71356278 | 97% |
反応手順
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%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08552039B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-688984c870574770a6a80db22151b732 |
| 出典メモ | uspto-grants-2013_10 |