反应详情

Into a 50 l enamelled double-walled apparatus equipped with a stirrer and adjusted to azeotropic distillation 7.5 kg (0.125 kmole) of n-propanol, 19 kg of benzene, 25 kg (0.1 kmole) of 4-chloro-3,5-dinitro-benzoic acid and 1 kg of concentrated sulfuric acid are weighed in. The reactor is closed and the content thereof is heated to boiling by means of steam heating. The reaction mixture is heated to boiling (86°-90° C. until no more water leaves the system while the organic phase (a mixture of benzene and n-propanol) is continuously reintroduced into the reactor. Once the distillation of water is completed (5-7 hours) the mixture is cooled below 20° C., the precipitated crystals are isolated by centrifugation, washed with cold benzene and dried. Thus 25.4 kg of the desired compound are obtained, yield 88%, purity 97%.

1. customequipped with a stirrer
2. customThe reactor is closed
3. temperaturethe content thereof is heated
4. temperatureheating
5. temperatureThe reaction mixture is heated
6. custom86°-90° C.
7. customleaves the system while the organic phase (
8. additionis continuously reintroduced into the reactor
9. distillationOnce the distillation of water
10. custom(5-7 hours)
11. temperatureis cooled below 20° C.
12. customthe precipitated crystals are isolated by centrifugation
13. washwashed with cold benzene
14. customdried