CONTINUOUS FLOW SYNTHESIS PROCESS FOR PHENYLHYDRAZINE SALT AND SUBSTITUTED PHENYLHYDRAZINE SALT

摘要

Provided is a continuous flow synthesis process for a phenylhydrazine salt and a substituted phenylhydrazine salt. Three reactions, namely diazotization, reduction, and acid hydrolysis for salt formation, are organically integrated, an aniline or substituted aniline acid solution, a diazotized reagent, a reducing agent, and an acid serve as raw materials, a salt of a phenylhydrazine derivative is produced by means of the three reactions performed continually in turn of diazotization, reduction, and acid hydrolysis for salt formation. The synthesis process is performed in an integrated reactor and is an integrated solution. The reaction raw materials are continuously added through a material inlet of the integrated reactor, the reactions of diazotization, reduction, and acid hydrolysis for salt formation are performed continually in turn in the integrated reactor, and the salt of the phenylhydrazine derivative is produced continuously at a material outlet of the integrated reactor, the total reaction time being 20 min. Compared with a conventional production process, the total reaction time is greatly reduced, the degree of safety is significantly increased, also, both the reaction process and the reaction product comprise no reaction by-product (such as a diazoamino compound or a reduction reaction intermediate), the continuous flow process comprises no additional purification step and produces high-purity products with a purity of 99% or more.