CN1706783A - Synthesis process of 1,2,3-trimethoxy benzene - Google Patents
Synthesis process of 1,2,3-trimethoxy benzene Download PDFInfo
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- CN1706783A CN1706783A CN 200510018690 CN200510018690A CN1706783A CN 1706783 A CN1706783 A CN 1706783A CN 200510018690 CN200510018690 CN 200510018690 CN 200510018690 A CN200510018690 A CN 200510018690A CN 1706783 A CN1706783 A CN 1706783A
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Abstract
The present invention provides synthesis process of 1, 2, 3-trimethoxyl benzene. The synthesis process of 1, 2, 3-trimethoxyl benzene includes: throwing pyrogallol, water and tetrabutyl ammonium bromide into reactor; dropping dimethyl sulfate and industrial liquid alkali; lowering the temperature to 20 deg.c for crystallization; centrifugally dewatering after finishing crystallization to obtain coarse 1, 2, 3-trimethoxyl benzene product; mixing the coarse product, alcohol and water in the weight ratio of 1 to 2 to 4 in the reactor; heating the mixture to 90 deg.c for crystallization; centrifugally dewatering to obtain refined 1, 2, 3-trimethoxyl benzene product; and rectification in rectifying reactor through electrically heating to obtain final product. The said synthesis process is simple and suitable for industrial production.
Description
Technical field:
The present invention relates to a kind of synthetic and preparation method of organic compound, particularly a kind of 1,2, the preparation method of 3-trimethoxy-benzene.
Background technology:
A kind of 1,2, the 3-trimethoxy-benzene is a Turkey-galls deep processed product, can be used for organic synthesis and pharmaceutical industry field, and is current, the method that does not also have industrial utilization pyrogallol to produce.
Summary of the invention:
The purpose of this invention is to provide a kind of 1,2, the synthesis technique of 3-trimethoxy-benzene.The present invention a kind of 1,2, the synthesis technique of 3-trimethoxy-benzene is characterized in that, is to put in reactor at 50: 100: 1 to stir with pyrogallol (pyrogallol), water, tetrabutyl phosphonium bromide ammonia by mass ratio, and after stirring the mixture evenly, per 151 kilograms mixture drips the industrial lye 90L of methyl-sulfate 125L and 30%, and the control reactor temperature is about 35 ℃, dropwised back insulation 3 hours, temperature remains on 30 ℃, is warming up to 95 ℃ and be incubated 2 hours again; Need be cooled to 20 ℃ of crystallizations 12～16 hours during the material crystallization; Treat that temperature drops to 20 ℃, centrifuge dehydration obtained 1,2 after crystallization was finished, and the crude product of 3-trimethoxy-benzene, moisture content are controlled at below 20%; Is to put in reactor at 1: 2: 4 to stir with crude product, ethanol, water by mass ratio, after stirring the mixture evenly, feeds steam and is warmed to 90 ℃, treat to cool to 5～10 ℃ of crystallizations 12～16 hours after material dissolution fully, centrifuge dehydration, moisture content are controlled at below 20%, obtain 1,2, the elaboration of 3-trimethoxy-benzene is put into elaboration in the rectifying still, and electrically heated heats up and distills, temperature is controlled at 130～132 ℃, obtains finished product.The present invention is a kind of 1,2, and the synthesis technique step of 3-trimethoxy-benzene is simple, and equipment requirements is low, is suitable for suitability for industrialized production.
Embodiment:
In actual production, 100 kilograms of pyrogallols (pyrogallol), 200 kg of water, 2 kilograms of tetrabutyl phosphonium bromide Dressed of measuring are put in the reactor and stir, after stirring the mixture evenly, drip the industrial lye 180L of methyl-sulfate 250L and 30%, and controlled temperature is about 35 ℃, dropwised back insulation 3 hours, temperature remains on 30 ℃, is warming up to 95 ℃ and be incubated 2 hours again; Need be cooled to 20 ℃ during the material crystallization; Treat that temperature dropped to 20 ℃ of crystallizations after 14 hours, centrifuge dehydration obtains 1,2, the crude product of 3-trimethoxy-benzene, and the moisture content of crude product is controlled at 18%; 100 kilograms of crude products, 200 kilograms of ethanol, 400 kg of water are put in the reactor and stirred, after stirring the mixture evenly, feed steam and be warmed to 90 ℃, treat to cool to 10 ℃ of crystallizations after material dissolution fully, in crystallization centrifuge dehydration after 14 hours, moisture content is controlled at 18%, obtains 1,2, the elaboration of 3-trimethoxy-benzene is put into elaboration in the rectifying still, and electrically heated heats up and distills, temperature is controlled at 131 ℃, obtains finished product.
Claims (1)
1, the present invention a kind of 1,2, the synthesis technique of 3-trimethoxy-benzene is characterized in that, is to put in reactor at 50: 100: 1 to stir with pyrogallol, water, tetrabutyl phosphonium bromide ammonia by mass ratio, and after stirring the mixture evenly, per 151 kilograms mixture drips the industrial lye 90L of methyl-sulfate 125L and 30%, and the control reactor temperature is about 35 ℃, dropwised back insulation 3 hours, temperature remains on 30 ℃, is warming up to 95 ℃ and be incubated 2 hours again; Need be cooled to 20 ℃ of crystallizations 12～16 hours during the material crystallization; Treat that temperature drops to 20 ℃, centrifuge dehydration obtained 1,2 after crystallization was finished, and the crude product of 3-trimethoxy-benzene, moisture content are controlled at below 20%; Is to put in reactor at 1: 2: 4 to stir with crude product, ethanol, water by mass ratio, after stirring the mixture evenly, feeds steam and is warmed to 90 ℃, treat to cool to 5～10 ℃ of crystallizations 12～16 hours after material dissolution fully, centrifuge dehydration, moisture content are controlled at below 20%, obtain 1,2, the elaboration of 3-trimethoxy-benzene is put into elaboration in the rectifying still, and electrically heated heats up and distills, temperature is controlled at 130～132 ℃, obtains finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100186904A CN100402479C (en) | 2005-05-09 | 2005-05-09 | Synthesis process of 1,2,3-trimethoxy benzene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100186904A CN100402479C (en) | 2005-05-09 | 2005-05-09 | Synthesis process of 1,2,3-trimethoxy benzene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1706783A true CN1706783A (en) | 2005-12-14 |
| CN100402479C CN100402479C (en) | 2008-07-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005100186904A Expired - Fee Related CN100402479C (en) | 2005-05-09 | 2005-05-09 | Synthesis process of 1,2,3-trimethoxy benzene |
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| CN (1) | CN100402479C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665417B (en) * | 2008-09-02 | 2012-08-15 | 中化宁波（集团）有限公司 | One-pot process for synthesizing 1,2,3-trimethoxy-benzene by using o-vanillin |
| CN102875344A (en) * | 2012-10-11 | 2013-01-16 | 常州华南化工有限公司 | Method for preparing 2, 3, 4-trimethoxybenzaldehyde |
| CN106631714A (en) * | 2016-08-30 | 2017-05-10 | 贝利化学（张家港）有限公司 | Method for synthesizing 2,6-dimethoxyphenol |
| CN106220477B (en) * | 2016-08-01 | 2019-01-18 | 湖南棓雅生物科技有限公司 | Gallic acid directly produces the technology of 1,2,3- trimethoxy-benzene |
-
2005
- 2005-05-09 CN CNB2005100186904A patent/CN100402479C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665417B (en) * | 2008-09-02 | 2012-08-15 | 中化宁波（集团）有限公司 | One-pot process for synthesizing 1,2,3-trimethoxy-benzene by using o-vanillin |
| CN102875344A (en) * | 2012-10-11 | 2013-01-16 | 常州华南化工有限公司 | Method for preparing 2, 3, 4-trimethoxybenzaldehyde |
| CN102875344B (en) * | 2012-10-11 | 2016-05-11 | 常州华南化工有限公司 | A kind of preparation method of 2,3,4-TMB |
| CN106220477B (en) * | 2016-08-01 | 2019-01-18 | 湖南棓雅生物科技有限公司 | Gallic acid directly produces the technology of 1,2,3- trimethoxy-benzene |
| CN106631714A (en) * | 2016-08-30 | 2017-05-10 | 贝利化学（张家港）有限公司 | Method for synthesizing 2,6-dimethoxyphenol |
| CN106631714B (en) * | 2016-08-30 | 2019-04-23 | 贝利化学（张家港）有限公司 | A method of synthesis 2,6- syringol |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100402479C (en) | 2008-07-16 |
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Granted publication date: 20080716 Termination date: 20110509 |