The research aims to optimize the synthesis process of oxyfluorfen, improve the product yield and purity, and turn byproducts into wealth. According to an original process
route,
resorcinol is used as a starting
raw material, and oxyfluorfen is synthesized through double etherification,
nitration and
ether exchange. After optimization, the total yield reaches 94.1%, and the purity reaches 98.4%. In order to improve the
utilization rate of the raw materials, an acidic water phase obtained after
quenching of an oxyfluorfen reaction solution is subjected to reduced pressure
distillation, the byproduct 3-chloro-4-hydroxy-
trifluorotoluene is recovered, and the yield can reach 93.7%. Further serving as a
raw material of a new process, and synthesizing a target product through
nucleophilic substitution. In the
route, 2, 4-dichloronitrobenzene with moderate reaction activity and better selectivity is innovatively used for replacing 2, 4-difluoronitrobenzene, so that
side reaction is effectively inhibited, and a target product with the content of 98.7% is obtained at the total yield of 94.8%. According to the new and old
combination strategy, through integration of two process routes, high-valued conversion of by-products is realized, limitation of a traditional synthesis method is broken through, and
atom economy is remarkably improved.