Chloroform → 3-(4,5-dichloro-1H-imidazol-2-yl)pyridine
반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[NH:8]C=[CH:10][N:11]=2)[CH:2]=1.[Cl:12]N1C(=O)CCC1=O.[CH:20]([Cl:23])(Cl)Cl>>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[NH:8][C:20]([Cl:23])=[C:10]([Cl:12])[N:11]=2)[CH:2]=1참가 물질
4
실험 절차
To a suspension of 2-(3-pyridyl)-imidazole (1.5 g., 0.01 moles) in chloroform (150 ml.) is added dropwise with stirring over one hour at reflux N-chlorosuccinimide (2.6 g., 0.02 moles). The reaction mixture is heated three hours at reflux. After cooling, the solvent is removed at 20 mm. and the residue triturated with water while heating on a steam bath. The resulting solid is filtered and after recrystallization from acetonitrile 400 mg. of 2-(3-pyridyl)-4,5-dichloroimidazole is obtained, m.p. 237°-238° C.
후처리
- additionis added dropwise
- temperatureThe reaction mixture is heated three hours
- temperatureat reflux
- temperatureAfter cooling
- customthe solvent is removed at 20 mm
- customand the residue triturated with water
- temperaturewhile heating on a steam bath
- filtrationThe resulting solid is filtered
- customafter recrystallization from acetonitrile 400 mg
출처 및 근거
- ORD 기록
- ord-6b62ec7126eb43fb85506213ab94d354
- 출처 데이터셋
- uspto-grants-1977_11
- 특허 번호
- US04058614
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