Synthesis method of 2, 4-butane sultone

Abstract

The invention discloses a synthesis method of 2, 4-butane sultone, which comprises the following steps: 1, dissolving 1, 3-propane sultone in a first organic solvent under the protection of inert gas in the whole process, then adding sodium hydrogen in batches, and heating to 40-50 DEG C after the sodium hydrogen is added; 2, dropwise adding a methylation reagent, and carrying out heat preservation reaction after dropwise adding; and 3, cooling to room temperature, adding ice water and a second organic solvent for extraction, and carrying out negative pressure rectification on the second organic solvent layer to obtain the final product 2, 4-butane sultone. The synthesis method has the advantages of low raw material cost, simple operation steps, mild reaction conditions, few reaction steps, easiness in purification and the like.

Description

technical field [0001] The invention relates to the technical field of synthesis of sultone derivatives, in particular to a synthesis method of 2,4-butane sultone. Background technique [0002] The application of sultone derivatives is very extensive, and the application fields include sizing and dyeing and finishing in the fuel industry and the textile industry, additives for lithium-ion battery electrolytes, and photosensitive materials. Therefore, a cheap and easy method is used to synthesize sultones Derivatives will have a considerable market space in the future. [0003] 2,4-butane sultone is a typical sulfoalkylation reagent. At present, the synthesis methods of 2,4-butane sultone mainly include the following types: [0004] The first synthesis method: first sulfonate butylene chloride with sulfur dioxide to chlorobutanesulfonic acid, then intramolecularly condense and dehydrochloride to 2,4-butane sultone; since the sulfonating agent sulfur dioxide is a gas, The re...

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Problems solved by technology

[0004] The first synthesis method: first sulfonate butylene chloride with sulfur dioxide to chlorobutanesulfonic acid, then intramolecularly condense and dehydrochloride to 2,4-butane sultone; since the sulfonating agent sulfur dioxide is a gas, The reaction conditions are harsh and the yield is low

[0005] The second synthesis method: use sodium bisulfite to sulfonate crotonaldehyde into sodium aldehyde butane sulfonate, then generate sodium hydroxybutane sulfonate under Raney nickel catalytic hydrogenation conditions, and then undergo acidification and high temperature intramolecular dehydration Generate 2,4-butane sultone; since the Raney nickel catalytic hydrogenation condition is high-pressure hydrogenation reduction, the reaction conditions are relatively harsh, and the follow-up operation is relatively cumbersome

[0006] The third synthesis method: first extract the hydrogen of 1,3-propane sultone with n-butyllithium, then add methyl bromide to generate 2,4-butane sultone; because n-butyllithium is relatively active, so The reaction temperature needs to be very low, and the equipment requirements are relatively strict; in addition, the methylation reagent methyl bromide is a gas at room temperature, and the safety performance is low and the operation is inconvenient.

[0007] In summary, the current synthetic methods of 2,4-butane sultone generally have problems such as harsh reaction conditions, cumbersome operation steps, long reaction steps, and low yields.