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Chloracetate water phase synthesis technology and novel method for preparing 2,4-D ester

A technology of chloroacetate and chloroacetic acid, applied in the field of preparation of 2,4-D ester, can solve the problems of high cost, long reaction time, complicated operation, etc., and achieves avoiding a large amount of use and waste, simple and convenient post-treatment process, good purity

Active Publication Date: 2016-12-21
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method needs to use organic solvent as water-carrying agent, needs to use catalyst, reaction time is long, operation is complicated, and cost is high

Method used

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  • Chloracetate water phase synthesis technology and novel method for preparing 2,4-D ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 Aqueous phase synthesis technology of methyl chloroacetate and preparation of 2,4-D methyl ester

[0041] Add 205g of methanol (6.4mol), 771.4g of chloroacetic acid (8mol) and 400g of water into a 2000mL three-neck flask equipped with a thermometer, a stirring device and a reflux device, mix and stir and heat up to 90°C, react for 6h, and stir and heat As well as the esterification reaction, the azeotropic system formed by methanol, methyl chloroacetate and water first passes through a reboiler with hot water at 78°C, and the methanol solution with a low boiling point passes through the reboiler and flows upward through condensation. In the reaction bottle, the high-boiling methyl chloroacetate solution is condensed and enters the water separator for stratification, the lower layer of methyl chloroacetate is released and collected, and the upper layer aqueous solution is pumped back into the reaction bottle.

[0042] Mix and stir 83.2g (0.5mol) of 2,4-dichloro...

Embodiment 2

[0043] Example 2 Aqueous Phase Synthesis Technology of Butyl Chloroacetate and Preparation of 2,4-D Butyl Ester

[0044] Add 185g of butanol (2.5mol), 241.1g of chloroacetic acid (2.5mol) and 300g of water into a 3000mL three-necked flask equipped with a thermometer, a stirring device and a reflux device, mix and stir and heat up to 120°C, react for 8 hours, and heat with stirring As well as the esterification reaction, the azeotropic system formed by butanol, butyl chloroacetate and water first passes through a reboiler with hot water at 125°C, and after the butanol and aqueous solution pass through the reboiler, they are condensed and flow back upwards. In the reaction bottle, the butyl chloroacetate with high boiling point is condensed and enters the water separator for stratification, the butyl chloroacetate in the lower layer is released and collected, and the azeotropic solution of the upper layer aqueous solution is pumped back into the reaction bottle.

[0045] 83.2g (...

Embodiment 3

[0046] Example 3 Aqueous Phase Synthesis Technology of Isooctyl Chloroacetate and Preparation of 2,4-D Isooctyl

[0047] Add 390g of isooctyl alcohol (3mol), 212.1g of chloroacetic acid (2.2mol) and 500g of water into a 3000mL three-necked flask equipped with a thermometer, a stirring device and a reflux device, mix and stir and raise the temperature to 150°C, and react for 7 hours. Heating and esterification reaction, the azeotropic system formed by isooctyl alcohol, isooctyl chloroacetate and water first passes through a reboiler at 110°C, and the aqueous alcohol solution passes through the reboiler, then flows upward through condensation and returns to the reaction bottle , the high-boiling isooctyl chloroacetate solution is condensed into the water separator for stratification, the lower layer of isooctyl chloroacetate is released and collected, and the upper layer aqueous solution is pumped back into the reaction bottle.

[0048] 83.2g (0.5mol) of 2,4-dichlorophenol, 300g...

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Abstract

The invention discloses a chloracetate water phase synthesis technology and a novel method for preparing 2,4-D ester, and belongs to the technical field of organic synthesis. According to the chloracetate water phase synthesis technology, alcohol and chloroacetic acid are used as raw materials for preparing chloracetate in the water phase. The method for preparing 2,4-D ester comprises the following steps that (1) chloracetate is prepared; (2) 2,4-dichloroindophenol sodium is prepared; (2) the chloracetate directly takes a reaction with 2,4-dichloroindophenol sodium under the alkaline condition to obtain the corresponding 2,4-D ester. The operation of the preparation method of the chloracetate provided by the invention is performed in the water phase, so that the purity of the obtained coarse ester is higher, and can reach 99.3 percent or higher only through simple distillation; the corresponding 2,4-D ester is prepared from the chloracetate; the preparation process of the 2,4-D ester is greatly simplified; the cost is effectively reduced; the reaction time is greatly shortened; in addition, the product yield is improved; the waste water quantity is effectively reduced; the green chemical industrial requirements are met.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, specifically relates to a chloroacetate aqueous phase synthesis technology and a new method for preparing 2,4-D ester, in particular to a method with high yield, high purity, high efficiency and simple process Preparation of 2,4-D esters. Background technique [0002] 2,4-D ester, namely 2,4-dichlorophenoxyacetate, belongs to phenoxyacetic acid hormone-type selective herbicides. Has strong systemic conductivity. Its structural general formula is as follows: [0003] [0004] Where R represents methyl, ethyl, butyl, isooctyl and other hydrocarbon groups. [0005] According to the investigation of the literature, the existing synthesis method of 2,4-D ester is mainly prepared by the esterification reaction of 2,4-D with the corresponding alcohol. However, the cost of this method is relatively high, and the amount of waste water in the existing preparation process of raw material 2,...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/63C07C67/343C07C69/712
CPCC07C37/66C07C67/08C07C67/343C07C69/63C07C69/712C07C39/44
Inventor 岳涛邢文国冯维春陈琦付永丰李培培游淇徐婷
Owner QINGDAO UNIV OF SCI & TECH
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