Ethyl acetate synthesis method

A technology of ethyl acetate and synthesis method, which is used in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of low yield, troublesome post-processing, easy-to-corrode equipment, etc., and achieve high yield , The effect of convenient post-processing and resource saving

CN109694325AInactive Publication Date: 2019-04-30张欣
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2019-04-30
Estimated Expiration
Not applicable · inactive patent
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Abstract

The invention relates to an ethyl acetate synthesis method, and belongs to the technical field of organic chemistry and pharmaceutical synthesis. The steps comprises: soaking a macroporous cation exchange resin sequentially with acetic acid, sodium hydroxide and acetic acid, rinsing with water after soaking, making the pH value of the resin achieve a neutral state, filtering, and removing the water adhered to the surface of the macroporous cation exchange resin to obtain a pre-treated resin; and pouring acetic acid and the pre-treated resin into toluene, carrying out an esterification reactionwhile adding an organic acid ethyl ester in a dropwise manner, filtering after completing the reaction to separate the resin, filtering the toluene liquid after cooling the toluene liquid so as to obtain unreacted acetic acid, washing the ethyl acetate toluene liquid with water, carrying out pressure reducing condensation, recovering the solvent through, and distilling to obtain the ethyl acetate. According to the present invention, the synthesis method has advantages of high yield, convenient post-treatment, no pollution and recycling, wherein the resin can be directly reused, and the solvent is recovered and applied, such that the resources can be saved, and the environmental protection can be achieved.
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Description

technical field

[0001] The invention belongs to the technical field of organic chemistry and medicine synthesis, in particular to a method for synthesizing ethyl acetate. Background technique

[0002] Ethyl acetate is 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. Ethyl acetate and its derivatives, as a class of important organic intermediates, are widely used in the technical field of pharmaceutical synthesis.

[0003] At present, domestic related synthesis methods have disadvantages such as difficult control of the amount of reactants, many side reactions, low yield, and troublesome post-treatment. At the same time, the catalysts used include concentrated sulfuric acid, hydrochloric acid, p-toluenesulfonic acid, triethylamine, and methanol. Sodium and liquid c...

Examples

Embodiment 1

[0022] A) Resin pretreatment, first soak the styrene-based macroporous cation exchange tree in the order of acetic acid soaking, sodium hydroxide soaking and acetic acid soaking again, and rinse with deionized water after each soaking, specifically: first Immerse the styrene series macroporous cation exchange resin with a hydrochloric acid solution with a mass percent concentration of 3%, wherein the weight ratio of the 3% hydrochloric acid solution to the styrene macroporous cation exchange resin is 5:1, The soaking time is 150min. After soaking, the hydrochloric acid solution is exhausted, that is, the acid solution is exhausted and rinsed to pH7 with deionized water, and then soaked in a sodium hydroxide solution with a mass percentage concentration of 3%. The sodium hydroxide solution and benzene The weight ratio of ethylene macroporous cation exchange resin is 5: 1, and the soaking time of sodium hydroxide is 150min. Rinse to pH10, then soak 150min with the hydrochloric a...