Synthesis method of 1,4-butane sultone

A technology of butane sultone and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of many by-products, difficult to control operation mode, etc., achieve high total yield, ensure high and low temperature storage performance, and reduce side reactions. Effect

Active Publication Date: 2019-05-21
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The existing operation mode of this method is not easy to control, the reaction yield is only about 60%, and there are many by-products, the purity is about 99.9%, the moisture > 150ppm, and the acid value > 150ppm

Method used

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  • Synthesis method of 1,4-butane sultone
  • Synthesis method of 1,4-butane sultone
  • Synthesis method of 1,4-butane sultone

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Preparation of chlorobutyl acetate

[0031] Put 196g of tetrahydrofuran and 42g of zinc powder into the reaction bottle, install a reflux device, stir in an ice-water bath to cool down to below 15°C, start to add 48g of acetyl chloride dropwise, and finish adding in 3 hours. After heat preservation at 60°C for 2 hours, the reaction was completed, and 388.8 g of the intermediate chlorobutyl acetate was recovered under reduced pressure, with a yield of 95%.

[0032] Preparation of 1,4-butane sultone

[0033] Drop into intermediate chlorobutyl acetate 151g, sodium sulfite 190g, water 360g in the reaction bottle, install reflux device, stir and heat reflux, timing 16h, solution becomes clear, reaction finishes, extract part of water under reduced pressure until there is solid to separate out, cool down to Below 45°C, add methanol hydrochloride (41.9%, 300ml) dropwise, stir for 2 hours, cool down to 5°C, and filter with suction. To 130°C, 1-3mmHg high-vacuum decompression ...

Embodiment 2

[0036] Preparation of chlorobutyl acetate

[0037] Put 73g of tetrahydrofuran and 85g of zinc powder into the reaction bottle, install a reflux device, stir in an ice-water bath to cool down to below 15°C, start to add 86g of acetyl chloride dropwise, and the dropwise addition is completed in 2.5 hours. Keep warm at 60°C for 1.5h, the reaction is over, and 142.67g of intermediate chlorobutyl acetate is extracted under reduced pressure, with a yield of 93.8%.

[0038] Preparation of 1,4-butane sultone

[0039] Put 142g of the above-mentioned intermediate chlorobutyl acetate, 220g of sodium sulfite, and water into the reaction flask until sodium sulfite is a saturated solution, install a reflux device, stir and heat to reflux, and count for 15 hours, the solution becomes clear, the reaction is over, and part of the water is extracted under reduced pressure When there is solid precipitation, cool down to below 45°C, add dropwise methanol hydrochloride (41.9%, until the pH value ...

Embodiment 3

[0042] Preparation of chlorobutyl acetate

[0043] Put 145g of tetrahydrofuran and 160g of zinc powder into the reaction bottle, install a reflux device, stir in an ice-water bath to cool down to below 15°C, start to add 175g of acetyl chloride dropwise, and finish the dropwise addition in 2 hours. After the reaction was completed at 60°C for 1 hour, 285.2 g of the intermediate chlorobutyl acetate was recovered under reduced pressure, with a yield of 94.2%.

[0044] Preparation of 1,4-butane sultone

[0045] Put 151g of the above-mentioned intermediate chlorobutyl acetate, 252g of sodium sulfite, and water into the reaction bottle until the sodium sulfite is a saturated solution, install a reflux device, stir and heat to reflux, and count for 14 hours. When there is solid precipitation, lower the temperature to below 45°C, add dropwise methanol hydrochloride (41.9%, until the pH value is 3.2), stir for 1 hour, cool down to 4°C, filter with suction, the filter cake is the by-pro...

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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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/06
CPCY02E60/10
Inventor 葛建民刘鹏武利斌
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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