Method for synthesizing N,N'-dicyclohexylcarbodiimide by taking oxygen gas as oxidant

Abstract

The invention provides a method for synthesizing N,N'-dicyclohexylcarbodiimide by taking oxygen gas as an oxidant. The method comprises the following steps: adding N,N'-dicyclohexylthiourea into a high-pressure reaction kettle and taking n-hexane as a solvent; adding a V2O5-P2O5 catalyst; introducing enough oxygen gas and controlling pressure and temperature to carry out oxidization reaction for 2to 3h; then cooling to 15 DEG C and carrying out extraction filtration; and de-coloring, decompressing and distilling to obtain DCC. The method takes the oxygen gas as the oxidant and has high reaction selectivity and low dangers; meanwhile, the generation amount of wastewater is greatly reduced and the wastewater is easy to treat; the problems of a traditional technology that the amount of wastesaline water is great and the waste saline water is difficult to treat are solved; a reaction system is optimized, the V2O5-P2O5 catalyst is used and the reaction is carried out in a homogeneous reaction system and is easy to control; the reaction yield is improved, the oxidization yield of the DCC reaches 93 percent or more and the purity of the DCC reaches 99.2 percent or more; and the method has the advantages that technological steps are green and environmentally friendly, the environment-protection investment is reduced and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and in particular relates to a method for synthesizing N,N'-dicyclohexylcarbodiimide by using oxygen as an oxidant. Background technique [0002] N,N'-Dicyclohexylcarbodiimide (DCC) is a good low-temperature biochemical dehydrating agent, used for the synthesis and dehydration of amikacin and amino acids, and also for the dehydration of acids, anhydrides, aldehydes, ketones, etc. Synthesis, this product is also used in the synthesis of peptides and nucleic acids. DCC dehydration condensation is used, the reaction conditions are mild, and the synthesis yield is high, so it is often used as a dehydrating agent or carboxyl activator for polypeptide synthesis, or for coupling small molecular compounds and polypeptides with carrier proteins. In recent years, the sales situation of DCC has continued to grow, and the supply of products is in short supply. At the same time, the pressu...

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Problems solved by technology

[0007] The purpose of the present invention is to provide a method for synthesizing N,N'-dicyclohexylcarbodiimide using oxygen as an oxidant, the process steps are safe and reliable, the reaction yield and product purity are high, and it solves the problem that the amount of waste brine in the traditional process is difficult to handle question