Preparation method of carbonyl diimidazole

Abstract

The invention discloses a preparation method of carbonyl diimidazole in the technical field of carbonyl diimidazole synthesis. The preparation method comprises the steps of taking imidazole and hexamethyl disilazane as starting materials, obtaining N-trimethylsilyl imidazole through condensation, absorbing a single byproduct, namely ammonia through a sodium hydroxide solution, allowing N-trimethylsilyl imidazole to react with triphosgene to prepare carbonyl diimidazole, and filtering the principal product, namely carbonyl diimidazole, from liquid trimethylchlorosilane for vacuum drying. A removal step is simpler; the byproduct is gaseous and does not influence purity of the product, namely N-trimethylsilyl imidazole; a reactor with higher purity is provided for a subsequent reaction; in areaction process of N-trimethylsilyl imidazole and triphosgene, no catalyst is required to be added; the method is simple to operate; a byproduct of the reaction of N-trimethylsilyl imidazole and triphosgene is liquid trimethylchlorosilane; and carbonyl diimidazole prepared by the method is higher in purity and good in quality.

Description

technical field [0001] The invention relates to the technical field of carbonyldiimidazole synthesis, and the specific field is a preparation method of carbonyldiimidazole. Background technique [0002] Carbonyldiimidazole is an imidazole derivative. It can be seen from structural analysis that there is a closed large P bond in its imidazole structure, and one of the nitrogen atoms is not bonded SP 2 There is a lone pair of electrons on the orbital, which determines that carbonyldiimidazole has strong chemical reactivity, and can react with functional groups such as ammonia, alcohol, acid, etc., and synthesize many compounds that are difficult to obtain by general chemical methods. Carbonyldiimidazole is widely used in Enzymes and protein binders, antibiotic synthetic drug intermediates, especially as bonding agents for the synthesis of polypeptide compounds. In recent years, through the research on carbonyldiimidazole as an activator, it has strong reactivity and wide appli...

AI Technical Summary

Problems solved by technology

[0002] Carbonyldiimidazole is an imidazole derivative. It can be seen from structural analysis that there is a closed large P bond in its imidazole structure, and one of the nitrogen atoms is not bonded SP 2 There is a lone pair of electrons on the orbital, which determines that carbonyldiimidazole has strong chemical reactivity, and can react with functional groups such as ammonia, alcohol, acid, etc., and synthesize many compounds that are difficult to obtain by general chemical methods. Carbonyldiimidazole is widely used in Enzymes and protein binders, antibiotic synthetic drug intermediates, especially as bonding agents for the synthesis of polypeptide compounds. In recent years, through the research on carbonyldiimidazole as an activator, it has strong reactivity and wide application , the reaction process is low toxicity, the product purification is simple, especially for different functional groups with high selectivity, which is of great significance in the field of organic synthesis and polymers; the existing preparation methods of carbonyldiimidazole include phosgene route synthesis, many Using benzene, toluene, and tetrahydrofuran as solvents, phosgene and imidazole as raw materials, reacting at a certain temperature, removing impurities, and evaporating to obtain the product, the yield is 70% to 80%. This method has a low yield and low product purity. The problem is that using imidazole and aromatic carbonate as raw materials, carbonyldiimidazole can also be obtained by reacting under a certain temperature and pressure and under the action of a catalyst, but the by-products of this method are difficult to remove, resulting in low product purity. Therefore, the above two methods All there is the shortcoming that product quality is not good, for this reason, propose a kind of preparation method of carbonyldiimidazole