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Synthetic method of monomethyl adipate

A technology of monoethyl adipate and synthesis method, which is applied in the field of synthesis of monoethyl adipate, can solve problems such as unstable chemical properties of adipic anhydride, easily corroded equipment, and pollute the environment, and achieve convenient post-processing, Resource saving and high yield effect

Inactive Publication Date: 2013-01-30
SUZHOU FUSHILAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Chinese Invention Patent Application Publication No. CN102351691A discloses a synthesis method of monoethyl adipate. The preparation method of this patent scheme is the same as the second synthesis method above. Diic anhydride, and then alcoholysis reaction of adipic acid and ethanol to obtain monoethyl adipate, but due to the unstable chemical properties of adipic anhydride, it is necessary to prepare and use immediately (i.e. ready-to-use), and prepare adipic anhydride A large amount of concentrated sulfuric acid is required, and it is also easy to corrode equipment and pollute the environment.

Method used

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  • Synthetic method of monomethyl adipate
  • Synthetic method of monomethyl adipate
  • Synthetic method of monomethyl adipate

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Embodiment 1

[0029] A) Resin pretreatment, first soak the styrene-based macroporous cation exchange tree in the order of acid solution soaking, alkali solution soaking and acid solution soaking again, and rinse with deionized water after each soaking, specifically: First soak the styrene macroporous cation exchange resin with a hydrochloric acid solution with a mass percentage concentration of 3%, wherein the weight ratio of the hydrochloric acid solution with a mass percentage concentration of 3% to the styrene macroporous cation exchange resin is 5:1 , soaking time is 150min, drain the hydrochloric acid solution after the soaking is over, i.e. drain the acid solution and rinse with deionized water to pH7, then use a sodium hydroxide solution with a mass percentage concentration of 3% for soaking, the sodium hydroxide solution and The weight ratio of styrene-based macroporous cation exchange resin is 5: 1, and the soaking time of alkali solution is 150min. After soaking in alkali solution,...

Embodiment 2

[0032] A) Resin pretreatment, be that the hydrochloric acid solution of 5% with mass percentage concentration is soaked to styrene series macroporous cation exchange resin earlier, wherein mass percentage concentration is the hydrochloric acid solution of 5% and styrene series macroporous cation exchange resin The weight ratio is 4:1, and the soaking time is 210min. After the soaking, the hydrochloric acid solution is exhausted, that is, the acid solution is exhausted and the acid solution is rinsed with deionized water to pH5, and then soaked in a sodium hydroxide solution with a mass percentage concentration of 5%. The weight ratio of this sodium hydroxide solution and styrene series macroporous cation exchange resin is 4: 1, and the time of lye soaking is 210min, and after lye immersion is finished, the sodium hydroxide solution is exhausted and the lye is exhausted, and again Rinse with deionized water to pH 7, then soak again for 210 minutes with 5% hydrochloric acid solut...

Embodiment 3

[0035] A) Resin pretreatment, be that the hydrochloric acid solution of 4% is soaked to styrene series macroporous cation exchange resin with mass percent concentration earlier, wherein mass percent concentration is the hydrochloric acid solution of 4% and styrene series macroporous cation exchange resin The weight ratio is 3:1, and the soaking time is 180min. After soaking, the hydrochloric acid solution is exhausted, that is, the acid solution is drained and the pH is rinsed with deionized water to pH6, and then soaked in a sodium hydroxide solution with a mass percentage concentration of 4%. The weight ratio of this sodium hydroxide solution and styrene series macroporous cation exchange resin is 3: 1, and the time of lye soaking is 180min, and after lye immersion is finished, the sodium hydroxide solution is exhausted and the lye is exhausted, and again Rinse with deionized water to pH 8, and then soak for 180 minutes again with a hydrochloric acid solution with a concentra...

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Abstract

The invention discloses a synthetic method of monomethyl adipate, belonging to the technical field of organic chemistry and drug synthesis. The synthetic method disclosed herein comprises the following steps: firstly successively immersing macroporous cation exchange resin in acid solution, alkali liquor and acid solution, then washing the immersed macroporous cation exchange resin with water until the pH value of the resin is neutral, then filtering and removing the moisture attached to the surface of the macroporous cation exchange resin to obtain a pretreated resin; adding adipic acid and the pretreated resin in toluene, and conducting esterification with adding organic ethyl gallate dropwisely, filtering after reaction finished to separate the resin, filtering the toluene liquid after the toluene liquid is cooled to leach unreacted adipic acid, washing the monomethyl adipate toluene liquid, conducting reduced pressure condensation and recovering the solvent, and then conducting distillation to obtain the monomethyl adipate. According to the invention, the method has the advantages of high yield, convenient the post-treatment, no pollution, and reusability; and the resin can be directly reused, the solvent is recovered, thus the resource can be saved, and environmental protection property is achieved.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry and medicine synthesis, in particular to a method for synthesizing monoethyl adipate. Background technique [0002] The English name of monoethyl adipate is: Adipic acid monoethyl ester; the molecular formula is: C 8 h 14 o 4 ; Molecular weight: 174.2. It appears as a white or slightly pink crystalline solid at room temperature. Melting point: 28~29°C, boiling point: 285°C (760mmHg), refractive index: n 20 D 1.4390, relative density: 0.986. Insoluble in water, easily soluble in alcohol, ether and other organic solvents. Monoethyl adipate and its derivatives, as a class of important organic intermediates, are widely used in the technical field of pharmaceutical synthesis. [0003] The synthetic method of monoethyl adipate mainly contains following three kinds: [0004] One is to obtain monoethyl adipate (such as document Blaise; Koehler; Bulletin de la Societe Chimique deFrance; ...

Claims

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Application Information

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IPC IPC(8): C07C69/44C07C67/10
Inventor 丁建飞钱庆
Owner SUZHOU FUSHILAI PHARMA CO LTD
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