Synthesis and purification method of 4, 7-dichloroquinoline

Abstract

The present invention relates to the technical field of compound synthesis, and discloses a 4, 7-dichloroquinoline synthesis purification method, which comprises: S1, primary reaction: adding 7-chloro-4-hydroxyquinoline into 300 g of toluene, sequentially adding DMF and triphenylphosphine oxide, starting stirring, internally heating to a temperature of 79-90 DEG C, slowly adding phosphorus oxychloride or a toluene solution of phosphorus oxychloride in a dropwise manner, after the dropwise adding is completed, carrying out a reaction for 2-3 h, and cooling to a room temperature to obtain the 4, 7-dichloroquinoline. Continuously reacting until the TLC monitoring reaction is finished; s2, performing reduced pressure distillation, namely performing reduced pressure distillation on the reaction liquid in the S1. The method has the advantages of simple operation, high yield, no use of any reagent in the purification process, no introduction of new impurities, no special requirements on equipment, no environmental pollution, no introduction of an organic solvent, no pollution, and easy industrial production.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a synthesis and purification method of 4,7-dichloroquinoline. Background technique [0002] 4,7-Dichloroquinoline is an intermediate of the antimalarial drug chloroquine sulfate and chloroquine phosphate. When 4,7-dichloroquinoline is synthesized by traditional synthesis techniques, 4,5-dichloroquinoline isomers and other impurities are sometimes generated , resulting in reduced yield and difficult purification. [0003] The existing purification and refining methods generally adopt the method (1) recrystallization on the basis of the existing synthesis process, such as the reagents used include methanol, ethanol, toluene, dichloromethane, chloroform, etc., but the purification is difficult, low purity, Repeated recrystallization is required, the yield is low, and the environment is polluted (without any reagents); (2) Sublimation method, 4,7-dichloroquinoline and iso...

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies in the prior art, the invention provides a method for the synthesis and purification of 4,7-dichloroquinoline, which solves the problem that impurities such as 4,7-dichloroquinoline and isomers synthesized by traditional techniques will be sublimated together, requiring several Super sublimation requires high equipment requirements, requires professional sublimation devices, and requires high precision in temperature and vacuum, which cannot meet people's requirements.

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