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Sulfuric Acid → 3-(1,3-Dioxaindan-5-yl)propane-1-thiol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Safrole | HCID 5144 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | HCID 178418634 | HCID 178418634 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(1,3-Dioxaindan-5-yl)propane-1-thiol | HCID 19001619 | 66.4% |
反応手順
25 g of thioacetic acid was added to 53.5 g of safrole in portions, while stirring the mixture at a room temperature or under cooling with ice/water. The reaction was carried out for 30 minutes. A solution of 20 g of sodium hydroxide in a mixture comprising 100 ml of water and 200 ml of ethanol was added to the reaction mixture. The obtained mixture was heated under reflux for 20 minutes, cooled, neutralized with dilute sulfuric acid and extracted with 1 l of benzene. The extract was washed with water and the benzene layer was dried over anhydrous sodium sulfate and purified by silica gel column chromatography (hexane) to obtain 42.8 g of the title compound as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05292901 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-bc49ae4e5efa440f81f3746c1ac1f30b |
| 出典メモ | uspto-grants-1994_03 |