Synthesis method of 1,4-butylenesulfone

Abstract

The invention discloses a synthesis method of 1,4-butylenesulfone, and belongs to the technical field of medical intermediate synthesis. The synthesis method is characterized by comprising the following steps: adding hydrosulfite into water in advance, stirring to dissolve hydrosulfite to obtain a solution; then adding sodium sulfite to adjust the pH to 7.5-9; heating to a temperature of 45 to 55 DEG C, dropwise adding butenol within 10 to 20 minutes at an even speed, controlling the addition reaction temperature in a range of 60 to 70 DEG C, after the butanol is completely added, keeping on carrying out reactions for 20 to 30 minutes, then stopping reactions, cooling the temperature to the room temperature; wherein the mole ratio of butenol to hydrosulfite is 1:1.05-1:3; after cooling, dropwise adding acid into the system until the system turns acidic, stirring the solution for 50 to 70 minutes, adding alcohol to carry out crystallization, filtering to obtain a clarified solution, and subjecting the clarified solution to rectification to obtain 1,4-butylenesulfone. The synthesis method has the advantages that the steps are few, the yield is high, the side products and water can be recovered, and the environment pollution is little.

Description

technical field [0001] A method for synthesizing 1,4-butane sultone belongs to the technical field of pharmaceutical intermediate synthesis. Background technique [0002] 1,4-Butane sultone is an important chemical and pharmaceutical intermediate, which can be used in the synthesis of photosensitive materials, surfactants, sulfonating agents and dye sensitizers. In addition, the power battery additive made of 1,4-butane sultone can reduce the embedding of the battery solvent to the electrode, prolong the life of the electrode, improve the power cycle efficiency, increase the number of battery cycles, and increase the battery life. [0003] In the prior art, 1,4-butane sultone is mainly synthesized by the following method. [0004] 1) 1,4-butane sultone is prepared by four-step reaction using tetrahydrofuran and acetyl chloride. The synthesis steps are many, the total yield is 45%, and there are many side reactions and by-products, so the industrial value is not great ; ...

AI Technical Summary

Problems solved by technology

[0009] 2) Using chlorobutane and thionyl chloride as raw materials to prepare the product through a three-step reaction, but a large amount of currently worthless mesylate is produced, which is difficult to separate and purify, and the yield is about 30%;

[0010] 3) Preparation of 1,4-butane sultone with 1-n-butene in ether and dichloromethane system, the reaction will produce a large number of by-products, distillation separation is difficult, and the use of dangerous solvent ether, the final product The yield is also lower;

[0011] 4) Using dioxane and sulfur trioxide as raw materials to prepare products through 4-step reaction, this reaction not only produces solid waste barium sulfate, but also needs to carry out hydrogenation addition reaction in an autoclave, the reaction cycle is long and the equipment requirements are high

[0012] In the above methods, the reaction cycle is long, the equipment requirements are high, the by-products are more, the environmental pressure is high, and industrialization is difficult.