Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → 3-(1,3-Dioxaindan-5-yl)propane-1-thiol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Safrole | HCID 5144 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | HCID 178418634 | HCID 178418634 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-(1,3-Dioxaindan-5-yl)propane-1-thiol | HCID 19001619 | 66.4% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05292901 |
| 출처 데이터셋 | uspto-grants-1994_03 |
| ORD ID | ord-bc49ae4e5efa440f81f3746c1ac1f30b |
| 출처 메모 | uspto-grants-1994_03 |