反应详情

8 g. (0.05 moles) of α-cyano-phenylacetic acid are dissolved in 80 ml. of dichloromethane, 10.2 g. (0.05 moles) of phosphorous pentachloride are added and the mixture is stirred for 2 hours at the boiling point of the dichloromethane. The reaction is completed when the hydrochloric acid evolution ceases. The solvent is distilled off and the residue containing the obtained acid chloride and phosphoroxychloride is taken up in carbontetrachloride and the solution is added dropwise to 13 g. (0.05 moles) of pentachlorophenol and 4 ml. (0.05 moles) of pyridine dissolved in 200 ml. of carbontetrachloride. The reaction mixture is cooled and the precipitated pyridine chlorohydrate is removed by washing twice with 50 ml. of water, dried, distilled off and the residue is distilled off with diisopropyl ether. The precipitated crystalline product is cooled and filtered. The α-cyanophenylacetic acid pentachlorophenyl ester is air-dried.

1. distillationThe solvent is distilled off
2. additionthe residue containing the obtained acid chloride and phosphoroxychloride
3. additionthe solution is added dropwise to 13 g
4. temperatureThe reaction mixture is cooled
5. customthe precipitated pyridine chlorohydrate is removed
6. washby washing twice with 50 ml
7. dry with materialof water, dried
8. distillationdistilled off
9. distillationthe residue is distilled off with diisopropyl ether
10. temperatureThe precipitated crystalline product is cooled
11. filtrationfiltered
12. dry with materialThe α-cyanophenylacetic acid pentachlorophenyl ester is air-dried