Preparing method for organic intermediate diacetoacetic acid (1,4-butanediol) ester

A technology of diacetoacetic acid and butanediol, applied in the directions of organic chemistry, ketene/polyketene preparation, etc., can solve the problems of difficult transesterification reaction, low product yield and the like, and achieves low cost, high product yield, The effect of less environmental pollution

Inactive Publication Date: 2014-05-28
NANTONG UNIVERSITY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] At present, its synthesis method is to carry out transesterification reaction with ethyl acetoacetate 1,4-butanediol, because the two hydroxyl groups in the 1,4-butanediol molecule are at both ends, it is not easy to carry out transesterification reaction, and the product yield very low rate

Method used

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  • Preparing method for organic intermediate diacetoacetic acid (1,4-butanediol) ester

Examples

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Effect test

Embodiment 1

[0017] In a four-necked reaction flask equipped with an electric stirrer, a reflux condenser and a thermometer, add 18g of 1,4-butanediol, 18.5g of diketene, 0.5g of a polymerization inhibitor, 0.3g of a catalyst, and 30g of a solvent , install a reflux condenser and a thermometer, start the agitator, and start timing when the temperature rises to 85°C, and the reaction time is 8-14h. After the reaction is completed, the reactant is alkali-washed with 10-15% (mass) lye, the water phase is separated, and atmospheric distillation is carried out to reclaim the solvent and unreacted raw materials, and then the remaining reactant is subjected to vacuum distillation, namely A colorless and transparent liquid diacetoacetate (1,4-butanediol) ester product was obtained, and the yield of the product reached 91.18%.

Embodiment 2

[0019] In a four-necked reaction flask equipped with an electric stirrer, a reflux condenser and a thermometer, add 18g of 1,4-butanediol, 21g of diketene, 0.5g of inhibitor, 0.3g of catalyst, 30g of solvent, Install a reflux condenser and a thermometer, start the stirrer, and start timing when the temperature rises to 85°C, and the reaction time is 8-14h. After the reaction is completed, the reactant is alkali-washed with 10-15% (mass) lye, the water phase is separated, and atmospheric distillation is carried out to reclaim the solvent and unreacted raw materials, and then the remaining reactant is subjected to vacuum distillation, namely A colorless and transparent liquid diacetoacetate (1,4-butanediol) ester product was obtained, and the yield of the product reached 91.49%.

Embodiment 3

[0021] In the four-necked reaction flask equipped with electric stirrer, reflux condenser and thermometer, add 18g of 1,4-butanediol, 25.2g of diketene, 0.8g of inhibitor, 0.6g of catalyst, 30g of solvent , install a reflux condenser and a thermometer, start the agitator, and start timing when the temperature rises to 85°C, and the reaction time is 8-14h. After the reaction is completed, the reactant is alkali-washed with 10-15% (mass) lye, the water phase is separated, and atmospheric distillation is carried out to reclaim the solvent and unreacted raw materials, and then the remaining reactant is subjected to vacuum distillation, namely A colorless and transparent liquid (1,4-butanediol) diacetoacetate product was obtained, and the yield of the product reached 91.97%.

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Abstract

The invention discloses a preparing method for organic intermediate diacetoacetic acid (1,4-butanediol) ester, which includes the following steps: using ketene dimer and 1,4-butanediol as raw materials, and reacting to obtain the diacetoacetic acid (1,4-butanediol) ester after the addition of a catalyst, a polymerization inhibitor and a solvent. During the synthesis of the diacetoacetic acid (1,4-butanediol) ester, the separation and purification process is simple, the reaction time is short, the product yield reaches 91% above, the product purity is higher, the energy consumption is low, environmental pollution is low, the cost is low, and the preparing method is an ideal technology for the realization of industrial production.

Description

technical field [0001] The invention relates to a preparation method of an organic intermediate diacetoacetate (1,4-butanediol). Background technique [0002] Diacetoacetate (1,4-butanediol) ester is an important fine chemical raw material and organic synthesis intermediate, mainly used in the synthesis of non-toxic stabilizer 1,4-butanediol bis-β-amino croton for polyvinyl chloride Intermediates of acid esters. The chemical name is diacetoacetic acid (1,4-butanediol), and its molecular formula: C 12 h 18 o 6 , molecular weight: 258.26, molecular structure formula: [0003] [0004] Physical and chemical properties: Appearance is colorless liquid, boiling point: 101-104℃ / 2.33kPa. [0005] At present, its synthesis method is to carry out transesterification reaction with ethyl acetoacetate 1,4-butanediol, because the two hydroxyl groups in the 1,4-butanediol molecule are at both ends, it is not easy to carry out transesterification reaction, and the product yield The...

Claims

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Application Information

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IPC IPC(8): C07C69/72C07C67/46
CPCC07C67/46C07C69/72
Inventor 王树清高崇汤艳峰
Owner NANTONG UNIVERSITY
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