Thionyl Chloride → 5-(Chloromethyl)-1-Ethyl-1H-Imidazole Hydrochloride
반응식
[CH2:1]([N:3]1[C:7]([CH2:8]O)=[CH:6][N:5]=[CH:4]1)[CH3:2].S(Cl)([Cl:12])=O>>[ClH:12].[Cl:12][CH2:8][C:7]1[N:3]([CH2:1][CH3:2])[CH:4]=[N:5][CH:6]=1참가 물질
3
반응 조건
- 온도
- 90 °C
실험 절차
To 1-ethyl-5-hydroxymethylimidazole (9.5 g), thionyl chloride (50 ml) was added by portions at 0° C., and the mixture was heated for 30 minutes under nitrogen atmosphere at 90° C. The mixture was allowed to be at room temperature. The solvent was distilled off under reduced pressure and the obtained residue was dissolved in methanol, and the solvent was distilled off again under reduced pressure. The obtained solid was recrystallized from ethyl acetate, to give 5-chloromethyl-1-ethylimidazole hydrochloride (12.4 g) as colorless crystals.
후처리
- customto be at room temperature
- distillationThe solvent was distilled off under reduced pressure
- dissolutionthe obtained residue was dissolved in methanol
- distillationthe solvent was distilled off again under reduced pressure
- customThe obtained solid was recrystallized from ethyl acetate
출처 및 근거
- ORD 기록
- ord-230b7f53409948d0b950c5669e97b5db
- 출처 데이터셋
- uspto-grants-2007_08
- 특허 번호
- US07262185B2
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