Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzene → 2,7,9,9-Tetramethyl-1,4-dioxaspiro[4,5]dec-6-en-8-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzene | HCID 241 | — |
| 반응물 | Propylene Glycol | HCID 1030 | — |
| 반응물 | Ketoisophorone | HCID 62374 | — |
| 촉매 | p-Toluenesulfonic acid | HCID 6101 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2,7,9,9-Tetramethyl-1,4-dioxaspiro[4,5]dec-6-en-8-one | HCID 13209183 | 80% |
반응 단계
To a 2-liter flask fitted with a reflux condenser, a water separator and a stirrer is charged 265 g of 2,6,6-trimethylcyclohex-2-en-1,4-dione (prepared by the method described in Helv. Chim. Acta, 39:2041 [1956]), 266 g of propylene glycol, 500 ml of benzene and 1 g of p-toluenesulfonic acid. The reactants are stirred and refluxed until no additional water is collected in the water separator. The product is washed with water to a pH of 6, and the solvent is stripped off. The residue is vacuum distilled through a 9 inch Goodloe column to yield 257 g of product, boiling point 92° C. at 1 mm Hg (80% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04130508 |
| 출처 데이터셋 | uspto-grants-1978_12 |
| ORD ID | ord-fa8d2972bb6e4b3c9738f814b4025252 |
| 출처 메모 | uspto-grants-1978_12 |