반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([CH3:9])[CH:3]=1.[C:10]([C:14]1[CH:21]=[CH:20][C:17]([CH2:18]Cl)=[CH:16][CH:15]=1)([CH3:13])([CH3:12])[CH3:11].O>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:7]=[C:6]([CH2:18][C:17]2[CH:20]=[CH:21][C:14]([C:10]([CH3:13])([CH3:12])[CH3:11])=[CH:15][CH:16]=2)[C:5]([OH:8])=[C:4]([CH3:9])[CH:3]=1참가 물질
실험 절차
106.5 g (0.75 mol) 4-chloro-2-methylphenol and 45.67 g (0.25 mol) 4-tert. butylbenzylchloride are dissolved in 200 ml chloroform, and 22.5 g water-free zinc chloride are added as Friedel-Crafts catalyst. Thereafter the reaction mixture is stirred, whereby indeed at room temperature to the start of the reaction intense gas development, i.e. intense reaction, is to be noted. Subsequently the reaction mixture is stirred at 60° C. 5-6 h and washed three times each with 200 ml water for the purpose of removing the zinc chloride. The organic phase is dried across magnesium sulfate and the chloroform is driven off in a vacuum. At 182°-185° C./0.3 Torr the 4-chloro-2-methyl-6-(4'-tert. butylbenzyl)-phenol distills over as water-clear, viscous, nearly odorless liquid.
후처리
- customwhereby indeed at room temperature to the start of the reaction intense gas development, i.e. intense reaction
- stirringSubsequently the reaction mixture is stirred at 60° C
- wash5-6 h and washed three times each with 200 ml water for the purpose
- customof removing the zinc chloride
- dry with materialThe organic phase is dried across magnesium sulfate
- distillationAt 182°-185° C./0.3 Torr the 4-chloro-2-methyl-6-(4'-tert. butylbenzyl)-phenol distills over as water-clear
출처 및 근거
- ORD 기록
- ord-10fcae91893c403881b74948e7c2dc88
- 출처 데이터셋
- uspto-grants-1985_07
- 특허 번호
- US04532367
연결된 노트
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