Preparation of N-alkyl thiophosphoryl triamide by one-pot method

Abstract

The invention discloses a method for preparing N-alkyl thiophosphoryl triammonium through a favorable one-pot method in industry. The method is characterized in that in a tetrahydrofuran solvent, in the presence of a tertiary amine acid-binding agent, and at an reaction temperature of between 10 below zero and 50 DEG C, thiophosphoryl chloride and alkyl primary amine react to generate N-alkyl amino thiophosphoryl bichloride and tertiary amine acid-binding agent hydrochloride as intermediate products; the generated intermediate products continuously react with ammonia gas in the same reaction system without purification and separation to generate the N-alkyl thiophosphoryl triammonium, the acid-binding agent and ammonium chloride as target products; the target products are filtered and condensed to obtain the product; and the yield of the N-alkyl thiophosphoryl triammonium is more than or equal to 85 percent. The method has the advantages of compact preparation process, low cost, high yield and suitablility for scale industrialized production.

Description

Technical field The invention belongs to the technical field of chemical synthesis, and relates to a preparation method of N-hydrocarbyl thiophosphoryl triamine urease inhibitors, in particular to a novel industrially advantageous "one-pot method" for preparing urease inhibitor N-hydrocarbyl thiophosphorus The acyl triamide method. Background technique N-hydrocarbyl thiophosphoryl triamide is one of the effective soil urease inhibitors used in agriculture. The main research reports on the synthesis of such compounds include: In 1985, Jaroslav F. Kolc et al. first disclosed in US4530714 that N-hydrocarbyl thiophosphoryl triamide compounds have urease inhibitory activity. The addition of urea of ​​this type of compound can increase the utilization rate of urea, increase plant growth, and increase crop yields. . The patent also discloses the synthesis and preparation method of N-hydrocarbyl thiophosphoric triamide, that is, the two-step method ("two-pot method") is adopted to p...

AI Technical Summary

Problems solved by technology

The purpose of the present invention is to provide a one-step ("one-pot method") preparation process of a urease inhibitor N-hydrocarbyl thiophosphoryltriamide with simplified process, continuous, high efficiency, low cost, and recyclable solvent and acid-binding agent , to solve the problems of low yield, long working hours, high cost and many reaction steps in the prior art