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2,5-hexanedione synthesis method

A synthetic method, the technology of hexanedione, which is applied in 2 fields, can solve the problems of high cost and rare raw materials, and achieve the effects of easy acquisition, low technical cost and high yield

Inactive Publication Date: 2020-02-28
HUAIHUA JINXIN NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Current technology costs are high and raw materials are scarce

Method used

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  • 2,5-hexanedione synthesis method
  • 2,5-hexanedione synthesis method
  • 2,5-hexanedione synthesis method

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[0011] The present invention provides a kind of synthetic method of 2,5-hexanedione, adopts tert-butyl acetoacetate to react with chloroacetone under the action of alkali to generate tert-butyl 3-acetylmethylacetoacetate, then hydrolyzes under acidic condition, Deacidification gives 2,5-hexanedione,

[0012] The synthetic chemical formula of described 2,5-hexanedione is as follows:

[0013]

[0014] The general formula of the 2,5-hexanedione intermediate is as follows:

[0015]

[0016] Wherein, the base is selected from anhydrous carbonate, triethylamine, pyridine, and the acid is selected from sulfuric acid, hydrochloric acid, phosphoric acid and trifluoroacetic acid.

Embodiment 1

[0019] In a 2000 ml reactor, add 260 g tert-butyl acetoacetate, 145 g chloroacetone and 1000 g toluene, raise the temperature to 60-80 °C, add 150 kg triethylamine dropwise, and continue the reaction for 5 hours after the drop is complete. Cool, filter, and remove toluene to obtain 290 kg of product tert-butyl 3-acetylmethylacetoacetate with a yield of 90.6%, which is used for the next step reaction.

[0020] Add 500g of 20% sulfuric acid solution and 290g of the product from the previous step into a 1000-liter enamel reaction kettle, heat to 60-70°C for 8 hours, cool, extract with toluene, remove toluene, and distill under reduced pressure to obtain 2,5-hexanedione 138kg, the yield is 90.9%.

Embodiment 2

[0022] In a 2000ml reactor, add 260g of tert-butyl acetoacetate, 145g of chloroacetone and 1000Kg of toluene, raise the temperature to 60-80°C, add 150kg of triethylamine dropwise, continue to react for 8 hours after the addition, cool and filter. Toluene was removed to obtain 280 kg of tert-butyl 3-acetylmethylacetoacetate with a yield of 87.5%. for the next reaction.

[0023] Add 500g of 20% hydrochloric acid solution and 290g of the product from the previous step into a 1000-liter enamel reaction kettle, heat to 60-70°C for 8 hours, cool, extract with toluene, remove toluene, and distill under reduced pressure to obtain 2,5-hexanedione 135kg, the yield is 90.3%.

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Abstract

The invention provides a 2,5-hexanedione synthesis method, which comprises: carrying out a reaction on tert-butyl acetoacetate and chloroacetone under the action of an alkali to generate tert-butyl 3-acetylmethyl acetoacetate, hydrolyzing under acidic conditions, and deacidifying to obtain 2,5-hexanedione. According to the invention, the method has beneficial effects of low technical cost, easilyavailable raw materials and high yield.

Description

【Technical field】 [0001] The invention relates to the technical fields of electronic materials and medicine, in particular to a synthesis method of 2,5-hexanedione. 【Background technique】 [0002] 2,5-Hexanedione is an electronic material and a pharmaceutical intermediate, usually obtained by hydrolysis of 2,5-dimethylfuran under the action of a catalyst. Another synthetic method is to react sodium ethyl acetoacetate with pure iodine to generate diethyl diacetylsuccinate, and then hydrolyze it with 10% sodium hydroxide solution. Current technology costs are high and raw materials are scarce. 【Content of invention】 [0003] The invention discloses a synthesis method of 2,5-hexanedione, so as to solve the problems involved in the background technology. [0004] To achieve the above object, the technical solution of the present invention is: [0005] A method for synthesizing 2,5-hexanedione, using tert-butyl acetoacetate to react with chloroacetone under the action of a b...

Claims

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Application Information

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IPC IPC(8): C07C67/313C07C69/716C07C45/67C07C45/65C07C49/12
CPCC07C67/313C07C45/676C07C45/65C07C69/716C07C49/12
Inventor 王有名
Owner HUAIHUA JINXIN NEW MATERIAL CO LTD
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