Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzene → Methyl 1,4-dioxaspiro[4.5]decane-8-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzene | HCID 241 | — |
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | Methyl 4-oxocyclohexanecarboxylate | HCID 226643 | — |
| 용매 | Ethylene Glycol | HCID 174 | — |
| 생성물 | Methyl 1,4-dioxaspiro[4.5]decane-8-carboxylate | HCID 10845708 | — |
반응 단계
A mixture of 189.7 g. of 4-carbomethoxy-1-cyclohexanone [3] (obtained as in Example 2B) in 2000 ml. of benzene, 67.5 ml. of ethylene glycol and 2.7 g. of p-toluenesulfonic acid is heated at reflux under a Dean-Stark trap for about 5 hours. After cooling, the solution is washed with saturated aqueous sodium bicarbonate and brine. The oily residue remaining when the organic solvent is evaporated to dryness and is distilled under vacuum to give 231.8 g. of 4-carbomethoxy-1-cyclohexanone ethylene ketal[4] having a boiling point of 95° to 100° C. at 0.30 mm. of Hg.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US03953425 |
| 출처 데이터셋 | uspto-grants-1976_04 |
| ORD ID | ord-bc727e796e42464d8a74f9326d6e4c73 |
| 출처 메모 | uspto-grants-1976_04 |