Synthesis method of 1,4-butane sultone

Abstract

The invention relates to a synthesis method of 1,4-butane sultone and belongs to the technical field of compound synthesis. The synthesis method takes tetrahydrofuran and acetylchloride as raw materials and comprises the following steps: A, preparation of butylchloroacetate: placing tetrahydrofuran and zinc powder in a container, cooling to 15 DEG C or lower, beginning to dropwise add acetylchloride, after dropwise adding, heating to 45 DEG C, holding the temperature for 8-10 hours, then heating to 60 DEG C, holding the temperature for 1-2 hour, performing pressure reduction to extract butylchloroacetate, and B, preparation of 1,4-butane sultone: allowing butylchloroacetate, sodium sulfite and water to give a heating reflux reaction for 14-16 hour, performing pressure reduction till a solid is separated out, cooling to 45 DEG C or lower, dropwise adding methanol hydrochloride solution, performing stirring for 1-2 hours, cooling to 4-6 DEG C, performing suction filtration, performing pressure reduction on filtrate to extract methanol, water and acetic acid, then heating to 130 DEG C, performing high vacuum pressure reduction cyclization for 0.5-1 hour, heating to 150 DEG C, and thenperforming high vacuum pressure reduction to extract 1,4-butane sultone. The synthesis method is simple; a reaction process is mild and stable; a prepared target product is high in yield and purity,and very low in water content and acid content.

Description

technical field

[0001] The invention belongs to the technical field of compound synthesis, and relates to a synthesis method of 1,4-butane sultone. The synthesis method of the invention is simple and easy to operate, the chemical reaction is mild and stable, the side reaction is less, the yield is high, and the obtained product has high purity . Background technique

[0002] 1,4-butane sultone is a colorless liquid at room temperature, with a melting point of 12.5-14.5°C, a boiling point of 134-136°C (0.53kPa), and a relative density of 1.331. 1,4-butane sultone can Miscible with many organic solvents, insoluble in water. 1,4-butane sultone can be widely used in the production and manufacture of pharmaceutical intermediates, daily chemicals, photosensitive materials, electroplating intermediates, and lithium batteries. As 1,4-butane sultone is developed and applied in wider and wider fields, especially in new energy lithium battery electrolytes, its market demand is increa...

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