참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Phenol | HCID 996 | — |
| 반응물 | 1-Dodecanethiol | HCID 8195 | — |
| 반응물 | 3,3,5-Trimethylcyclohexanone | HCID 13398 | — |
| 생성물 | (1,1'-Biphenyl)-2,3'-diol | HCID 33665 | — |
반응 단계
7.5 mol (705 g) phenol and 0.15 mol (30.3 g) dodecylthiol are introduced into a 1-liter round-bottomed flask equipped with a stirrer, dropping funnel, thermometer, reflux condenser and gas inlet pipe and saturated with dry HCl gas at 28° to 30° C. A solution of 1.5 mol (210 g) dihydroisophorone (3,3,5-trimethylcyclohexan-1-one) and 1.5 mol (151 g) phenol is added dropwise to the resulting solution over a period of 3 hours, HCl gas continuing to be passed through the reaction solution. After the addition, HCl gas is introduced for another 5 hours. The mixture is then left to react for 8 hours at room temperature. The excess phenol is then removed by steam distillation. The residue is hot-extracted twice with petroleum ether (60-90) and once with methylene chloride and filtered off. Yield: 370 g, Mp: 205°-207° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05227458 |
|---|
| 출처 데이터셋 | uspto-grants-1993_07 |
|---|
| ORD ID | ord-d1b6ca327397496489c9a50fd43663c3 |
|---|
| 출처 메모 | uspto-grants-1993_07 |
|---|