METHODS OF PRODUCING 1,5,7-TRIAZABICYCL4,4,0-DEC-5-ENE FROM REACTION OF DISUBSTITUTED CARBODIIMIDE AND DIPROPYLENE TRIAMINE

摘要

FIELD: chemistry.;SUBSTANCE: invention relates to versions of an improved method of producing 1,5,7-triazabicyclo[4,4,0]-dec-5-ene. Compound is used for an electrodeposition coating composition and for making a coated substrate by electrophoretic deposition onto a substrate of said composition. Method includes steps (a) forming a mixture containing disubstituted carbodiimide, dipropylene triamine, as well as a solvent based on ether and/or alcohol; and (b) heating said mixture at temperature from 160 °C to 240 °C to provide conditions of reaction of said disubstituted carbodiimide with said dipropylene triamine. Optionally step (c), on which a by-product is distilled from reaction mixture at step (b), wherein step (c) and step (b) are simultaneous. Preferably step a) is performed in alcohol, for example 2-butoxyethanol, monobutyl ether of diethylene glycol, polyol hexaethoxylated bisphenol A or a combination thereof. Version of method of producing 1,5,7-triazabicyclo[4,4,0]-dec-5-ene is conducting steps (a) of forming a mixture, containing disubstituted carbodiimide and dipropylene triamine; and (b) heating said mixture at a temperature of 160 °C to 240 °C to provide reaction of said disubstituted carbodiimide with said dipropylene triamine. Optionally step c) is carried out, wherein said heating is carried out while adding a diluent after step (b). Said method is implemented in absence of solvent based on ether and/or alcohol. Disubstituted carbodiimide represents is dialkyl carbodiimide, for example, N,N′-diisopropyl carbodiimide, N,N′-dicyclohexyl carbodiimide or combination thereof, or diaryl carbodiimide, for example, di-p-tolylcarbodiimide. Step a) in both versions of method can be carried out in presence of a subacid catalyst.;EFFECT: method increases degree of conversion (more than 90 %) and selectivity of process (100 %) to obtain desired product with high output for a short reaction time.;17 cl, 7 ex