Synthesis method of high-purity phthalic acid n-pentyl isoamyl ester

A technology of n-pentyl isopentyl ester and phthalic acid, which is applied to the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of carboxylic acid halides, to achieve easy control of the reaction, mild reaction conditions, and simple requirements for reaction equipment Effect

Inactive Publication Date: 2019-05-24
SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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At present, the synthesis research report of n-pentyl

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  • Synthesis method of high-purity phthalic acid n-pentyl isoamyl ester

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Embodiment 1

[0023] A process for synthesizing n-pentyl isopentyl phthalate, the steps are as follows:

[0024] (1) Prepare a 3L glass reactor, first add n-amyl alcohol (595g, 6.75mol), phthalic anhydride (1.0kg, 6.75mol), 1.0L pyridine in sequence, stir and dissolve, there is an exothermic phenomenon, heat up, The internal temperature is controlled at 60-65°C for 3 hours of ripening. After the reaction is over, add the reaction solution into 2L of water, add concentrated hydrochloric acid dropwise while stirring, adjust the pH value of the reaction solution to 1-2, and then use dichloromethane (3L×3) extraction, the combined organic phase, the organic phase was successively washed with 1N HCl solution (3L×2), water (3L×1), saturated sodium chloride solution (3L×1), dried over magnesium sulfate (200g), Concentrate to obtain 1.5kg white solid intermediate I, yield: 94%.

[0025] (2) Prepare a 5L glass reaction kettle and tail gas recovery device: first add 2.25L thionyl chloride and 1.5kg ...

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Abstract

The invention discloses a synthesis method of high-purity phthalic acid n-pentyl isoamyl ester. The method is characterized in that pyridine is adopted as alkali, and phthalic anhydride is adopted tobe reacted with n-pentanol to obtain an intermediate I; heating backflowing reaction is conducted on the prepared intermediate I and thionyl chloride, and intermediate II is obtained through depressurizing and distilling; purified intermediate II is added to dichloromethane to be reacted with isopentanol at room temperature, triethylamine is taken as alkali, a target coarse product is obtained after a series of treatments of layering, extracting, washing, drying, filtering and the like are conducted on the reactant after reaction, finally fraction of 162-165 DEG C/2 mmHg is collected after depressurizing distillation is conducted to obtain the high-purity phthalic acid n-pentyl isoamyl ester. The purity of the prepared high-purity phthalic acid n-pentyl isoamyl ester can reach up to 99% orabove, and the yield is 60% or above.

Description

technical field [0001] The invention relates to a method for high-purity n-pentyl isopentyl phthalate, which belongs to the technical field of synthesis of new organic materials and pharmaceutical intermediate applications. Background technique [0002] N-pentyl isopentyl phthalate is an important fine organic chemical product and organic intermediate, widely used in food additives, synthetic heat-stable materials, preparation of new material additives, etc., and used in the research and development of new pharmaceuticals, At present, it is mainly used as a plasticizer for cellulose resin, polymethyl methacrylate, polystyrene and chlorinated rubber. With the continuous development of economy and science and technology, the market demand for n-pentyl isopentyl phthalate will increase year by year. Therefore, it is very important to develop a method for synthesizing high-purity n-pentyl isopentyl phthalate and to realize industrialization. At present, the synthesis research ...

Claims

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Application Information

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IPC IPC(8): C07C69/80C07C67/14C07C67/58C07C67/54C07C69/78C07C67/08C07C67/313
Inventor 阚洪柱姜苏徐久振
Owner SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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