Synthesis process of di-tert-butyl dicarbonate

Abstract

The invention discloses a synthesis process of di-tert-butyl dicarbonate. According to the synthesis process, tert-butyl alcohol alkali metal salt and a carbonyl chloride compound are used as reactionraw materials; supercritical carbon dioxide is used as a reaction raw material and a solvent; and synthesis of the di-tert-butyl dicarbonate is carried out in a carbon dioxide supercritical state; the problem that no proper solvent exists in each step of reaction for producing di-tert-butyl dicarbonate is thoroughly solved by utilizing the super-strong solubility and permeability of the supercritical carbon dioxide, the carbon dioxide is used as both the reaction raw material and reaction solvent, so that the reaction is easier, the reaction temperature is increased to room temperature or above, and no side reaction exists; the supercritical carbon dioxide has different solubilities for a product and a by-product, so that the product is directly separated from the by-product, and the problems of post-treatment water pollution and product loss are avoided.

Description

technical field [0001] The invention belongs to the field of organic synthesis and relates to di-tert-butyl dicarbonate, in particular to a synthesis process and device for di-tert-butyl dicarbonate. Background technique [0002] Di-tert-butyl dicarbonate (also known as di-tert-butyl pyrocarbonate) is an amino-protecting agent in the process of organic synthesis. It is mostly used in the synthesis of chemicals such as special proteins, polypeptide drugs, and amino-containing organic intermediates. It has High activity, easy detachment, low cost and other advantages. There are two main types of synthesis techniques about di-tert-butyl dicarbonate. One is prepared by using mono-tert-butyl carbonate alkali metal salt and carbonyl chloride compounds as raw materials; the other is prepared by using mono-tert-butyl carbonate alkali metal salt and aromatic or aliphatic sulfonyl chloride compounds as raw materials. [0003] The gas phosgene method was used for di-tert-butyl dicarb...

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Problems solved by technology

In fact, diphosgene and triphosgene are still first converted into phosgene to participate in the reaction during the reaction process, so the solvent for the reaction cannot use alcohols such as tert-butanol that have a high solubility for raw materials and intermediates, and phosgene also exists The reaction temperature of the method system is low and the system is viscous, which leads to problems such as incomplete reaction, low yield, and difficult separation.

The inventors of these above-mentioned patents increase the solubility of tert-butanol alkali metal salt and mono-tert-butyl carbonate alkali metal salt by selecting different solvents or even multiple solvents to mix, thereby making phosgene (liquid phosgene, solid phosgene) participate in The reaction is easier and more thorough, but it is not very ideal at present, so some people add phase transfer catalyst to the system to improve the reaction activity, which increases the difficulty of subsequent product separation and wastewater treatment

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