반응식
Br[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Mg].[Cl:9][C:10]1[C:15]([C:16]#N)=[CH:14][CH:13]=[CH:12][N:11]=1.Cl.CC[O:21]CC>>[C:16]([C:15]1[C:10]([Cl:9])=[N:11][CH:12]=[CH:13][CH:14]=1)(=[O:21])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1참가 물질
실험 절차
A solution of 3.14 g (0.02 mols) bromobenzene in anhydrous ether is added dropwise to a suspension of 0.02 mols magnesium in anhydrous ether. The mixture is refluxed 1.5 hr. and is then cooled until room temperature. Now a solution of 1:38 g 2-chloro-3-cyanopyridine in 25 ml anhydrous ether is added slowly while stirring. The reaction mixture is refluxed 24 hrs. and there is added, after standing, 10% aqueous HCl. The aqueous layer is separated and the ethereal layer is washed with 25% aqueous HCl. The combined washings and the first aqueous layer are basified with 40% NaOH and extracted with ether. The combined extracts are dried (MgSO4) and solvent evaporated. The crude is distilled in vacuo. Yield: 0.8 g of title product, identical with that described in Ex. 1b.
후처리
- temperatureThe mixture is refluxed 1.5 hr
- temperatureThe reaction mixture is refluxed 24 hrs
- additionand there is added
- customThe aqueous layer is separated
- washthe ethereal layer is washed with 25% aqueous HCl
- extractionextracted with ether
- dry with materialThe combined extracts are dried (MgSO4) and solvent
- customevaporated
- distillationThe crude is distilled in vacuo
출처 및 근거
- ORD 기록
- ord-80a9d39b6da5471295ee1aa8da9ea37a
- 출처 데이터셋
- uspto-grants-1988_04
- 특허 번호
- US04736037
연결된 노트
불러오는 중…