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Hydrochloric Acid → 2-(3,4-Dimethoxyphenyl)-m-dithiane-2-propionic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,3-Propanedithiol | HCID 8013 | — |
| 反応物 | 4-(3,4-Dimethoxyphenyl)-4-oxobutanoic acid | HCID 219390 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-(3,4-Dimethoxyphenyl)-m-dithiane-2-propionic acid | HCID 22758398 | — |
反応手順
50 g of 3-veratroylpropionic acid in 400 ml of chloroform and 22.7 g of 1,3-propanedithiol are treated with hydrogen chloride up to saturation while stirring. After 3 hours at room temperature, the solution is evaporated to 50 ml and diluted with ether. The resulting solution is extracted three times with 5% sodium carbonate. The basic phases are combined and made acidic with concentrated hydrochloric acid. The precipitated product is extracted with ether/methylene chloride (1:3). The organic extracts are dried and evaporated. The residue is recrystallized from ethanol, there being obtained 2-(3,4-dimethoxyphenyl)-m-dithiane-2-propionic acid of melting point 134°-135° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04073797 |
| 出典データセット | uspto-grants-1978_02 |
| ORD ID | ord-308226929d674e2fbb82491970a75b93 |
| 出典メモ | uspto-grants-1978_02 |