反应详情

To a cooled solution of 150 g 2-chloro-nicotinoyl chloride in 400 ml benzene there is added slowly 238 g AlCl3. After refluxing 2 hrs. the reaction mixture is added with stirring to a slightly acidic ice: water mixture. The organic layer is separated and the aqueous one is extracted with ethyl ether. The combined organic layers are washed with HONa 1N, then with water, and dried over Na2SO4. The excess benzene is distilled at water pump pressure in a rotary evaporator and the residual oil is distilled in vacuo. Yield: 157 g of title product, b.p. 123° C./0.05 mm; m.p. 35°-7° C.; UV (ethanol): λmax. 254 nm., ε: 17,180; Cl 15.97 (16.29).

1. temperatureAfter refluxing 2 hrs
2. additionthe reaction mixture is added
3. customThe organic layer is separated
4. extractionthe aqueous one is extracted with ethyl ether
5. washThe combined organic layers are washed with HONa 1N
6. dry with materialwith water, and dried over Na2SO4
7. distillationThe excess benzene is distilled at water pump pressure in a rotary evaporator
8. distillationthe residual oil is distilled in vacuo