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 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | (1,1'-Biphenyl)-2,3'-diol | HCID 33665 | — |
반응 단계
1692 g (18 mol) of phenol, 60.6 g (0.3 mol) of dodecylthiol and 420 g (3 mol) of dihydroisophorone (3,3,5-trimethylcyclohexan-1-one) are introduced into a stirring apparatus equipped with a stirrer, thermometer, reflux condenser and gas inlet pipe at 28°-30° C. Dry HCl gas is introduced into this solution over a period of 5 hours at 28°-30° C. The mixture is then left to react for about 10 h at 28°-30° C. When 95% of the ketone has been converted (examined by GC), 2.5 l of water are added to the reaction mixture and a pH value of 6 is adjusted by adding a 45% NaOH solution. The reaction mixture is stirred for one hour at 80° C. and then cooled to 25° C. The aqueous phase is decanted off and the remaining residue is washed with water at 80° C. The resulting crude product is filtered off and hot-extracted twice with n-hexane and twice with methylene chloride and then filtered. The residue is recrystallised twice from xylene.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05227458 |
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| 출처 데이터셋 | uspto-grants-1993_07 |
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| ORD ID | ord-44d3854980e7474cabb4290501e38724 |
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| 출처 메모 | uspto-grants-1993_07 |
|---|