反应详情

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.

1. temperatureThe mixture is refluxed 1.5 hr
2. temperatureThe reaction mixture is refluxed 24 hrs
3. additionand there is added
4. customThe aqueous layer is separated
5. washthe ethereal layer is washed with 25% aqueous HCl
6. extractionextracted with ether
7. dry with materialThe combined extracts are dried (MgSO4) and solvent
8. customevaporated
9. distillationThe crude is distilled in vacuo