反应详情

A mixture of 346 ml of chlorobenzene and 120 g of valeryl chloride is treated, at room temperature, in the course of 1 hour with portions of aluminium chloride and the mixture is at the same time heated to 70°. The mixture is stirred for a further hour at this temperature and then cooled to 25° and the dark red reaction mixture is poured on to 1,000 g of ice. Concentrated hydrochloric acid is added and the mixture is then extracted with ethyl acetate. The organic extract is washed with 2 N hydrochloric acid, filtered through a diatomaceous earth formulation (Hyflo) and washed with further 2 N hydrochloric acid, twice with water with a 2 N aqueous solution of sodium carbonate and with water. It is dried over sodium sulphate and filtered and the filtrate is evaporated under reduced pressure. The residue is distilled; 4-chloro-valerophenone is obtained at 155°-156°/14 mm Hg; the product crystallises and melts at 28°-30°.

1. temperatureheated to 70°
2. temperaturecooled to 25°
3. customthe dark red reaction mixture
4. extractionthe mixture is then extracted with ethyl acetate
5. extractionThe organic extract
6. washis washed with 2 N hydrochloric acid
7. filtrationfiltered through a diatomaceous earth formulation (Hyflo)
8. washwashed with further 2 N hydrochloric acid, twice with water with a 2 N aqueous solution of sodium carbonate and with water
9. dry with materialIt is dried over sodium sulphate
10. filtrationfiltered
11. customthe filtrate is evaporated under reduced pressure
12. distillationThe residue is distilled