CN102863320B - Preparation technology of veratrole - Google Patents
Preparation technology of veratrole Download PDFInfo
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- CN102863320B CN102863320B CN201210405038.8A CN201210405038A CN102863320B CN 102863320 B CN102863320 B CN 102863320B CN 201210405038 A CN201210405038 A CN 201210405038A CN 102863320 B CN102863320 B CN 102863320B
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Abstract
The invention discloses a preparation technology of veratrole. The preparation technology comprises the steps as follows: taking the catechol as the main raw material, and catalyzing under the catalysis of a catalyst; taking the dimethyl sulfate as the methylating raw material, and carrying out the reaction; and then distilling to obtain the product. The product prepared by the preparation technology disclosed by the invention is stable in quality, and high in yield; the product has the yield over 99% based on the mol; the main content is more than 98.0% under efficient gas phase detection; and the product cannot be discolored by being positioned at room temperature for a long time.
Description
Technical field
The present invention is specifically related to a kind of preparation technology of veratrole.
Background technology
Veratrole, chemical name is 1,2-dimethoxy benzene, sterling is colourless transparent liquid, low temperature time be solid, fusing point 22-23 ℃, having industrial use widely, is a kind of important fine chemical material, is equally also one of important source material of a kind of compound essence and field of medicaments.Manufacturing enterprise is a lot of in the market, in order to occupy the market shares of putting into more, can only start with and improve yield and quality from technique.
The shortcoming that the preparation technology of veratrole in the past exists: process using pyrocatechol method, guaiacol method and o-chloro-anisole method in the past, above-mentioned several general yields all can only reach 93% left and right.
Summary of the invention
Object of the present invention adopts new catalyst, provides that a kind of purity is high, yield is high, the preparation technology of the veratrole of environmental protection.The present invention adopts Dodecyl trimethyl ammonium chloride to make the yield of original popular pyrocatechol method obtain the lifting of 5% left and right as the process reaction that methylates, and when having improved yield, and the lifting that quality is also passed through transformation efficiency is more than 99.5%.
The technical scheme of taking for the present invention that achieves the above object is:
In reaction vessel, add 1400L methyl-sulfate, open and stir, add 1000kg pyrocatechol; Add catalyzer Dodecyl trimethyl ammonium chloride, be warming up to 40 ℃, at 40-60 ℃, drip liquid caustic soda 1600L, after adding, at 50 ℃, stir 1h. and be warmed up to 70 ℃, control temperature at 70-90 ℃, add liquid caustic soda 900L, after adding, continue to be warming up to backflow, reflux temperature is 99 ℃ of left and right.Backflow 10h.After backflow finishes, standing 1h, separates lower aqueous layer.Oil reservoir adds liquid caustic soda water, and washing once.Obtain the thick oil of thick oily 1300 ㎏ left and right.Then thick oil is carried out more than underpressure distillation obtains finished product 1240 ㎏.Yield is more than 98.0%.
Preparation technology of the present invention, take pyrocatechol as body material, adds catalyzer, first through methyl-sulfate, methylates, then under alkaline condition, react, and, finally distill and obtain product.Constant product quality, yield is high.The above % of molar product yield 98.0, more than 99.5%, places also nondiscoloration for a long time through the efficient main content of vapor detection under product room temperature.
Embodiment
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
embodiment 1:in 5000L enamel reaction still, add 1400L methyl-sulfate, open and stir, add 1000kg pyrocatechol; Add catalyzer Dodecyl trimethyl ammonium chloride, with steam, be warming up to 40 ℃, at 40-60 ℃, drip liquid caustic soda 1600L, use during this time circulating water cooling, after adding, at 50 ℃, stir 1h. and be warmed up to 70 ℃, control temperature at 70-90 ℃, add liquid caustic soda 900L, after adding, continue to be warming up to backflow, reflux temperature is 99 ℃ of left and right.Backflow 10h.After backflow finishes, standing 1h, separates lower aqueous layer.Upper strata oil reservoir adds liquid caustic soda, and washing once.Obtain slightly oil of thick oily 1345 ㎏.Then thick oil is carried out to underpressure distillation and obtain finished product 1238 ㎏.Yield 98.6%.
Product is used the vertical 9790A gas chromatograph of good fortune to analyze, 150 ℃ of column temperatures, and 220 ℃ of detected temperatures, 220 ℃ of vaporization temperatures, adopt SE-30 pillar 30m * 0.32mm * 0.33 μ m, detect main content more than 99.5%.
Claims (1)
1. a preparation technology for veratrole, is characterized in that, comprises the steps:
In reaction vessel, add 1400L methyl-sulfate, open and stir, add 1000kg pyrocatechol; Add catalyzer Dodecyl trimethyl ammonium chloride, be warming up to 40 ℃, at 40-60 ℃, drip liquid caustic soda 1600L, after adding, at 50 ℃, stir 1h, be warmed up to 70 ℃, control temperature at 70-90 ℃, add liquid caustic soda 900L, after adding, continue to be warming up to backflow, reflux temperature is at 99 ℃ of left and right, backflow 10h; After backflow finishes, standing 1h, separates lower aqueous layer, and oil reservoir adds liquid caustic soda, and washing once, obtains thick oil, thick oil is carried out to underpressure distillation and obtain finished product veratrole.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210405038.8A CN102863320B (en) | 2012-10-23 | 2012-10-23 | Preparation technology of veratrole |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210405038.8A CN102863320B (en) | 2012-10-23 | 2012-10-23 | Preparation technology of veratrole |
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| Publication Number | Publication Date |
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| CN102863320A CN102863320A (en) | 2013-01-09 |
| CN102863320B true CN102863320B (en) | 2014-11-05 |
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| CN201210405038.8A Active CN102863320B (en) | 2012-10-23 | 2012-10-23 | Preparation technology of veratrole |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183588A (en) * | 2013-03-15 | 2013-07-03 | 张家港威胜生物医药有限公司 | Preparation method of veratrole |
| CN106518631B (en) * | 2016-09-07 | 2019-03-01 | 张家港威胜生物医药有限公司 | A kind of preparation method of veratrole |
| CN110054549A (en) * | 2019-04-12 | 2019-07-26 | 新昌县泰如科技有限公司 | A kind of preparation method of p-methyl anisole |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468943A (en) * | 2007-12-25 | 2009-07-01 | 南通莱嘉利化工有限公司 | Preparation technique of 1,6-dimethoxynaphthalene |
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- 2012-10-23 CN CN201210405038.8A patent/CN102863320B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468943A (en) * | 2007-12-25 | 2009-07-01 | 南通莱嘉利化工有限公司 | Preparation technique of 1,6-dimethoxynaphthalene |
Non-Patent Citations (2)
| Title |
|---|
| Vilsmeier法合成3, 4-二甲氧基苯甲醛的研究;王成峰等;《长沙电力学院学报(自然科学版)》;20041130;第19卷(第4期);第88页左栏第1.2 * |
| 王成峰等.Vilsmeier法合成3 4-二甲氧基苯甲醛的研究.《长沙电力学院学报(自然科学版)》.2004 * |
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| CN102863320A (en) | 2013-01-09 |
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Address after: 256651, No. nine, No. 99, Phoenix Road, Binhu District, Bincheng District, Shandong, Binzhou Patentee after: SHANDONG HOLLY PHARMACEUTICAL CO.,LTD. Address before: 256651, No. nine, No. 2, Phoenix Road, Binhu District, Bincheng District, Shandong, Binzhou Patentee before: Binzhou Hongrui Medical Technology Co.,Ltd. |
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Denomination of invention: Preparation process of resveratrol Effective date of registration: 20230626 Granted publication date: 20141105 Pledgee: Bank of Qingdao Co.,Ltd. Binzhou Branch Pledgor: SHANDONG HOLLY PHARMACEUTICAL CO.,LTD. Registration number: Y2023980045867 |
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