反应详情

A solution of 1.831 kg of 1,2,3-trichloro-4-nitrobenzene and 0.861 kg of copper cyanide in 1.21 L of DMF is heated to 155° C. for 2 hours, then cooled to room temperature. A solution of 3.24 kg of ferric chloride hexahydrate, 0.806 L of concentrated hydrochloric acid, and 4.87 L of water is added and the solution heated to 65° C. for 20 minutes. The mixture is cooled, stirred with 0.55 kg of charcoal and 4 L of toluene, and filtered. The organic phase is separated and the aqueous phase extracted with toluene. The combined toluene layers are washed with water and 6 N HCl, dried and concentrated to give a slurry. The slurry is dissolved in 1.5 L of methanol, and stored at 5° C. for 24 hours. The nitrile product is collected by filtration, washed with 1.5 L cold methanol and dried at 40° C.

1. temperaturethe solution heated to 65° C. for 20 minutes
2. temperatureThe mixture is cooled
3. filtrationfiltered
4. customThe organic phase is separated
5. extractionthe aqueous phase extracted with toluene
6. washThe combined toluene layers are washed with water and 6 N HCl
7. customdried
8. concentrationconcentrated
9. customto give a slurry
10. filtrationThe nitrile product is collected by filtration
11. washwashed with 1.5 L cold methanol
12. customdried at 40° C.