Hydrochloric Acid → Sepazonium chloride
반응식
Cl.[Br-].[Cl:3][C:4]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:5]=1[CH:6]([O:21][CH2:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:24]=1[Cl:30])[CH2:7][N+:8]1[CH:12]=[CH:11][N:10]([CH2:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:9]=1>CO>[Cl-:3].[Cl:3][C:4]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:5]=1[CH:6]([O:21][CH2:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:24]=1[Cl:30])[CH2:7][N+:8]1[CH:12]=[CH:11][N:10]([CH2:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:9]=1참가 물질
4
실험 절차
0.2 Mole of gaseous hydrogen chloride is dissolved in 32 parts of methanol and to this solution are added 12 parts of 1-[2,4-dichloro-β-(2,4-dichlorobenzyloxy)phenethyl]-3-phenethylimidazolium bromide. The resulting mixture is heated slowly to reflux temperature and stirred at reflux for 1.25 hours. The mixture is then cooled and evaporated, and the residue is triturated in n-hexane. The latter is decanted and the residual oil is boiled in methyl ethyl ketone, whereupon the desired product is precipitated as a solid. The latter is filtered off and crystallized from dioxane to obtain a purified 1-[2,4-dichloro-β-(2,4-dichlorobenzyloxy)phenethyl]-3-phenethylimidazolium chloride product, m.p. 159.5° C.
후처리
- temperatureThe resulting mixture is heated slowly
- temperatureto reflux temperature
- temperatureat reflux for 1.25 hours
- temperatureThe mixture is then cooled
- customevaporated
- customthe residue is triturated in n-hexane
- customThe latter is decanted
- customis precipitated as a solid
- filtrationThe latter is filtered off
- customcrystallized from dioxane
출처 및 근거
- ORD 기록
- ord-f3f16bbc64224c528fbd42e281fdb374
- 출처 데이터셋
- uspto-grants-1977_04
- 특허 번호
- US04017631
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