CN105622398A - Synthetic process of 2,4,6-trimethyl benzoic acid - Google Patents
Synthetic process of 2,4,6-trimethyl benzoic acid Download PDFInfo
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- CN105622398A CN105622398A CN201410584607.9A CN201410584607A CN105622398A CN 105622398 A CN105622398 A CN 105622398A CN 201410584607 A CN201410584607 A CN 201410584607A CN 105622398 A CN105622398 A CN 105622398A
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Abstract
The invention discloses a synthetic process of 2,4,6-trimethyl benzoic acid; 2,4,6-trimethyl benzoic acid can be used as an intermediate for dyes, insecticides, medicines and photoinitiators, and can be used for synthesizing trimethyl benzoyl chloride, a hardening agent for polyepoxide and a photoinitiator for a polymer. The synthetic process successively includes an acylation reaction, a chloroform reaction and a hydrolysis reaction and includes the following steps: (1), acylation reaction: taking sym-trimethylbenzene and chloroacethyl chloride as acylation raw materials, adopting an acylation catalyst, heating, filtering and acidifying the filtrate to prepare 2,4,6-trimethyl chloroacetophenone; (2), chloroform reaction: with the product obtained in the step (1) and sodium hypochlorite as raw materials, adopting a quaternary ammonium salt as a phase transfer catalyst, heating, carrying out a reduction reaction to prepare 2,4,6-trimethyl benzoic acid; and (3), hydrolysis reaction: carrying out extraction liquid dividing, acid neutralization and re-crystallization of the product obtained in the step (2).
Description
Technical field
The invention belongs to chemical process field, be specifically related to the synthesis technique of a kind of mesitylene carboxylic acid.
Background technology
The synthesis technique of 2,4,6-trimethylbenzoic acid at least includes the basic process such as haloform reaction, acylation reaction. In the synthesis technique of current mesitylene carboxylic acid, technological process is not easy to implement, and separation efficiency is low, it is impossible to achieve the recycling of raw material, and manufacturing process is complicated, and production efficiency is low.
Summary of the invention
For the above-mentioned technical problem overcoming prior art to exist, it is an object of the invention to, it is provided that the synthesis technique of a kind of mesitylene carboxylic acid, the present invention not only manufacturing process is simple, improve work efficiency, and achieves the guarantee of product quality.
The synthesis technique of mesitylene carboxylic acid provided by the invention, comprises the following steps:
(1) acylation reaction: with sym-trimethylbenzene. and chloracetyl chloride for acyl group raw material thing, adopts acyl group catalyst, prepares 2,4,6-trimethyl chloroacetophenones through steps such as intensification, filtration, acidification of filtrate, and preparation temperature controls at 220-380 DEG C;
(2) haloform reaction: with step (1) products therefrom and sodium hypochlorite for raw material, employing quaternary ammonium salt is phase transfer catalyst, through be warming up to 180-280 DEG C, reduction reaction step prepare mesitylene carboxylic acid;
(3) hydrolysis: namely step (2) gained reactant obtains end product then through extraction separatory, acid neutralization, recrystallization.
The synthesis technique of mesitylene carboxylic acid provided by the invention, it has the beneficial effects that, overcoming prior art, to prepare operation in mesitylene carboxylic acid process more, and the problem that workload is big improves work efficiency; Improve the utilization rate of catalyst.
Detailed description of the invention
Below in conjunction with an embodiment, the synthesis technique of mesitylene carboxylic acid provided by the invention is described in detail.
Embodiment
The synthesis technique of the mesitylene carboxylic acid of the present embodiment, comprises the following steps:
(1) acylation reaction: with sym-trimethylbenzene. and chloracetyl chloride for acyl group raw material thing, adopts acyl group catalyst, prepares 2,4,6-trimethyl chloroacetophenones through steps such as intensification, filtration, acidification of filtrate, and preparation temperature controls at 380 DEG C;
(2) haloform reaction: with step (1) products therefrom and sodium hypochlorite for raw material, employing quaternary ammonium salt is phase transfer catalyst, through be warming up to 180 DEG C, reduction reaction step prepare mesitylene carboxylic acid;
(3) hydrolysis: namely step (2) gained reactant obtains end product then through extraction separatory, acid neutralization, recrystallization.
The synthesis technique of mesitylene carboxylic acid, can directly prepare mesitylene carboxylic acid, it is not necessary to be processed further, and operation is simple, and measurement data is accurate, it is easy to implement.
Claims (1)
1. the synthesis technique of a mesitylene carboxylic acid, it is characterised in that: said method comprising the steps of:
(1) acylation reaction: with sym-trimethylbenzene. and chloracetyl chloride for acyl group raw material thing, adopts acyl group catalyst, prepares 2,4,6-trimethyl chloroacetophenones through steps such as intensification, filtration, acidification of filtrate, and preparation temperature controls at 220-380 DEG C;
(2) haloform reaction: with step (1) products therefrom and sodium hypochlorite for raw material, employing quaternary ammonium salt is phase transfer catalyst, through be warming up to 180-280 DEG C, reduction reaction step prepare mesitylene carboxylic acid;
(3) hydrolysis: namely step (2) gained reactant obtains end product then through extraction separatory, acid neutralization, recrystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410584607.9A CN105622398A (en) | 2014-10-28 | 2014-10-28 | Synthetic process of 2,4,6-trimethyl benzoic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410584607.9A CN105622398A (en) | 2014-10-28 | 2014-10-28 | Synthetic process of 2,4,6-trimethyl benzoic acid |
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| CN105622398A true CN105622398A (en) | 2016-06-01 |
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| CN201410584607.9A Pending CN105622398A (en) | 2014-10-28 | 2014-10-28 | Synthetic process of 2,4,6-trimethyl benzoic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110386868A (en) * | 2018-04-23 | 2019-10-29 | 天津墨森科技有限公司 | The preparation method of one kind 2,4,6- trimethylbenzoic acid |
| CN113387853A (en) * | 2021-06-15 | 2021-09-14 | 利民化学有限责任公司 | Method for preparing 2-chloro-3-methyl-4-methylsulfonylbenzoic acid |
-
2014
- 2014-10-28 CN CN201410584607.9A patent/CN105622398A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110386868A (en) * | 2018-04-23 | 2019-10-29 | 天津墨森科技有限公司 | The preparation method of one kind 2,4,6- trimethylbenzoic acid |
| CN113387853A (en) * | 2021-06-15 | 2021-09-14 | 利民化学有限责任公司 | Method for preparing 2-chloro-3-methyl-4-methylsulfonylbenzoic acid |
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Application publication date: 20160601 |