CN102452902A - Preparation method for phloroglucinol - Google Patents
Preparation method for phloroglucinol Download PDFInfo
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- CN102452902A CN102452902A CN 201010525455 CN201010525455A CN102452902A CN 102452902 A CN102452902 A CN 102452902A CN 201010525455 CN201010525455 CN 201010525455 CN 201010525455 A CN201010525455 A CN 201010525455A CN 102452902 A CN102452902 A CN 102452902A
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- benzene
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- phloroglucinol
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Abstract
The invention discloses a preparation method for phloroglucinol, comprising the following steps: mixing 1, 3, 5-trimethoxy benzene and concentrated hydrochloric acid or concentrated sulfuric acid, and adding H3PO4 into them, and stirring them for 24-48 h at room temperature; adding sodium carbonate into them in batches and neutralizing them, and regulating the pH value to 2-3 and filtering them; extracting the filter liquid by ether in batches, and drying the extraction liquid and evaporating out ether to obtain yellow solid phloroglucinol. The preparation method has an advantage of low production cost. The yield of the obtained phloroglucinol is higher than 80% and purity thereof is higher than 90%.
Description
Technical field:
The invention belongs to a kind of compound method of fine-chemical intermediate, particularly a kind of preparation method of Phloroglucinol.
Background technology:
Phloroglucinol is important organic synthesis intermediate, is mainly used in medical manufacturing field.1,3, the 5-trimethoxy-benzene is a kind of white crystalline powder, and is water insoluble.Preparation 1,3 at present, the method production cost of 5-trimethoxy-benzene is high, yield is generally less than 70%, and the total cost of the finished product is higher.
Summary of the invention:
The object of the invention just is to overcome the deficiency that exists in the above-mentioned prior art, and a kind of preparation method of Phloroglucinol is provided, and the production cost of this method is low, the yield of products obtained therefrom high.
As above design, technical scheme of the present invention is: a kind of preparation method of Phloroglucinol is characterized in that: with 1; 3,5-trimethoxy-benzene and concentrated hydrochloric acid or the vitriol oil mix the back and add H3PO4, after stirring at room 24-48 hour; Add the yellow soda ash neutralization in batches, pH value is transferred to the 2-3 after-filtration, it is batch extraction with ether to filtrate; The dry after-filtration of extraction liquid, steam ether, obtain the yellow solid Phloroglucinol.
Above-mentioned 1,3, the preparation method of 5-trimethoxy-benzene is: sodium Metal 99.5 and methanol mixed are made methanol solution of sodium methylate, add N then; With Cu2I2 and 1,3, the 5-tribromo-benzene adds, and is heated to 80-90 degree centigrade again; Stirring and refluxing reaction 2-3 hour is filtered, and filtrate decompression steams methyl alcohol and N, has steamed the back and has used steam distillation; Gained distillate crystallisation by cooling after-filtration, drying promptly get 1,3, the 5-trimethoxy-benzene.
Above-mentioned 1,3, the preparation method of 5-tribromo-benzene is: ethanol with 95% and benzene add 2,4,6-tribromo-benzene heating for dissolving after mixing again; In 1-2 hour time, progressively add the vitriol oil again, stir, add the back holding temperature at 50-60 degree centigrade; Add NaNO then in batches
2Boil insulation reaction 2-3 hour; Last cooling crystallization, filtration, water is washed till neutrality, is drying to obtain solid 1,3, the 5-tribromo-benzene.
Production cost of the present invention is low, the yield of gained Phloroglucinol is up to more than 80%, and purity reaches more than 90%.
Embodiment:
A kind of preparation method of Phloroglucinol, carry out according to the following step:
1, after being mixed, 95% ethanol and benzene adds 2,4 again, 6-tribromo-benzene heating for dissolving; In 1-2 hour time, progressively add the vitriol oil again, stir, add the back holding temperature at 50-60 degree centigrade; Add NaNO then in batches
2Boil insulation reaction 2-3 hour; Last cooling crystallization, filtration, water is washed till neutrality, is drying to obtain solid 1,3, the 5-tribromo-benzene.
2,10g sodium Metal 99.5 and 80ml methanol mixed are made methanol solution of sodium methylate, add the 80ml N then, again with 2gCu2I2 and 20g1,3; The 5-tribromo-benzene adds, and is heated to 90 degrees centigrade, and stirring and refluxing reaction 3 hours is filtered; Filtrate decompression steams methyl alcohol and N, has steamed the back and has used steam distillation, gained distillate crystallisation by cooling after-filtration, drying; Promptly get 1,3, the 5-trimethoxy-benzene.
3, with 3g1,3,5-trimethoxy-benzene and 200ml concentrated hydrochloric acid or the vitriol oil mix the back and add H3PO4; After stirring at room 24-48 hour; Add the neutralization of 120g yellow soda ash in batches, pH value is transferred to the 2-3 after-filtration, it is batch extraction with the 300ml ether to filtrate; The dry after-filtration of extraction liquid, steam ether, obtain the yellow solid Phloroglucinol.
Claims (3)
1. the preparation method of a Phloroglucinol is characterized in that: with 1,3; 5-trimethoxy-benzene and concentrated hydrochloric acid or the vitriol oil mix the back and add H3PO4, after stirring at room 24-48 hour, add the yellow soda ash neutralization in batches; PH value is transferred to the 2-3 after-filtration; It is batch extraction with ether to filtrate, and the dry after-filtration of extraction liquid, steams ether, obtains the yellow solid Phloroglucinol.
2. the preparation method of a kind of Phloroglucinol according to claim 1 is characterized in that: above-mentioned 1,3, the preparation method of 5-trimethoxy-benzene is: sodium Metal 99.5 and methanol mixed are made methanol solution of sodium methylate; Add N then, again with Cu2I2 and 1,3, the 5-tribromo-benzene adds; Be heated to 80-90 degree centigrade, stirring and refluxing reaction 2-3 hour is filtered; Filtrate decompression steams methyl alcohol and N, has steamed the back and has used steam distillation, gained distillate crystallisation by cooling after-filtration, drying; Promptly get 1,3, the 5-trimethoxy-benzene.
3. the preparation method of a kind of Phloroglucinol according to claim 1 is characterized in that: above-mentioned 1,3, the preparation method of 5-tribromo-benzene is: ethanol with 95% and benzene add 2,4,6-tribromo-benzene heating for dissolving after mixing again; In 1-2 hour time, progressively add the vitriol oil again, stir, add the back holding temperature at 50-60 degree centigrade; Add NaNO then in batches
2Boil insulation reaction 2-3 hour; Last cooling crystallization, filtration, water is washed till neutrality, is drying to obtain solid 1,3, the 5-tribromo-benzene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010525455 CN102452902A (en) | 2010-10-29 | 2010-10-29 | Preparation method for phloroglucinol |
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| CN 201010525455 CN102452902A (en) | 2010-10-29 | 2010-10-29 | Preparation method for phloroglucinol |
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| CN102452902A true CN102452902A (en) | 2012-05-16 |
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| CN 201010525455 Pending CN102452902A (en) | 2010-10-29 | 2010-10-29 | Preparation method for phloroglucinol |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012069A (en) * | 2012-12-30 | 2013-04-03 | 湖南尔康制药股份有限公司 | Production process of medicinal phloroglucinol |
| CN103641687A (en) * | 2013-11-30 | 2014-03-19 | 开封明仁药业有限公司 | Preparation method of phloroglucinol |
| CN106866378A (en) * | 2016-12-20 | 2017-06-20 | 上海昕盛医药科技有限公司 | A kind of synthesis technique of phloroglucin |
| CN109053382A (en) * | 2018-08-06 | 2018-12-21 | 国药集团化学试剂有限公司 | A kind of preparation method of phloroglucin |
| CN109180436A (en) * | 2018-09-14 | 2019-01-11 | 湖北凌晟药业有限公司 | A kind of synthetic method of phloroglucin |
| CN109369350A (en) * | 2018-11-23 | 2019-02-22 | 深圳市第二人民医院 | The synthetic method of Buflomedil Hydrochloride intermediate 1,3,5- trimethoxy-benzene |
| CN109400447A (en) * | 2018-11-13 | 2019-03-01 | 科利生物科技（徐州）有限公司 | The preparation method of pyrogallol |
| CN113527064A (en) * | 2021-08-03 | 2021-10-22 | 沈阳双鼎制药有限公司 | Preparation method of phloroglucinol |
-
2010
- 2010-10-29 CN CN 201010525455 patent/CN102452902A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012069A (en) * | 2012-12-30 | 2013-04-03 | 湖南尔康制药股份有限公司 | Production process of medicinal phloroglucinol |
| CN103012069B (en) * | 2012-12-30 | 2014-01-15 | 湖南尔康制药股份有限公司 | Production process of medicinal phloroglucinol |
| CN103641687A (en) * | 2013-11-30 | 2014-03-19 | 开封明仁药业有限公司 | Preparation method of phloroglucinol |
| CN103641687B (en) * | 2013-11-30 | 2015-06-17 | 开封明仁药业有限公司 | Preparation method of phloroglucinol |
| CN106866378A (en) * | 2016-12-20 | 2017-06-20 | 上海昕盛医药科技有限公司 | A kind of synthesis technique of phloroglucin |
| CN106866378B (en) * | 2016-12-20 | 2020-06-26 | 上海宏冠医药科技有限公司 | Synthetic process of phloroglucinol |
| CN109053382A (en) * | 2018-08-06 | 2018-12-21 | 国药集团化学试剂有限公司 | A kind of preparation method of phloroglucin |
| CN109180436A (en) * | 2018-09-14 | 2019-01-11 | 湖北凌晟药业有限公司 | A kind of synthetic method of phloroglucin |
| CN109400447A (en) * | 2018-11-13 | 2019-03-01 | 科利生物科技（徐州）有限公司 | The preparation method of pyrogallol |
| CN109369350A (en) * | 2018-11-23 | 2019-02-22 | 深圳市第二人民医院 | The synthetic method of Buflomedil Hydrochloride intermediate 1,3,5- trimethoxy-benzene |
| CN109369350B (en) * | 2018-11-23 | 2021-10-19 | 深圳市第二人民医院 | Synthesis method of buflomedil hydrochloride intermediate 1,3, 5-trimethoxybenzene |
| CN113527064A (en) * | 2021-08-03 | 2021-10-22 | 沈阳双鼎制药有限公司 | Preparation method of phloroglucinol |
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Application publication date: 20120516 |