CN101899019A - Method for producing medical raw material DM by using oxydol as oxidant - Google Patents
Method for producing medical raw material DM by using oxydol as oxidant Download PDFInfo
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- CN101899019A CN101899019A CN2010101285556A CN201010128555A CN101899019A CN 101899019 A CN101899019 A CN 101899019A CN 2010101285556 A CN2010101285556 A CN 2010101285556A CN 201010128555 A CN201010128555 A CN 201010128555A CN 101899019 A CN101899019 A CN 101899019A
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Abstract
The invention discloses a method for producing a medical raw material DM by using oxydol as an oxidant, which comprises the following steps of: adding water and a rubber accelerator M into a reaction kettle in a weight ratio of 1-15:1; adding sodium hydroxide into the reaction kettle in a molar ratio of 1:1-3 with the rubber accelerator M; adding M sodium salt liquid generated after reaction into an oxidation kettle, and adding a solvent (water, ethanol, methanol, isopropyl alcohol, acetone, aniline, toluene and the like) into the oxidation kettle in a volume ratio of 1:1-10 with the M sodium salt liquid; under the condition that the temperature is between 40 and 70 DEG C, dropping mixed oxidant solution of which the weight ratio of sulfuric acid to the oxydol is 1:1-12 into the mixture at a flow rate of 50 to 110 ml/minute, and stopping dropping the mixed oxidant when the pH of the solution is 4 to 8; and performing suction filtration, water washing, filtration and drying to obtain a product of the medical raw material DM, wherein the yield of the medical raw material DM is over 95 percent. The method has the following advantages that: sodium sulfate in the water can be reclaimed; the water and the isopropyl alcohol can be recycled; the method accords with a national environmental protection policy; and the purity of the medical raw material DM can reach 99 percent, and the melting point can be over 178 DEG C.
Description
Technical field
The present invention relates to the production method of a kind of medical material curing benzene a pair of horses going side by side thiazole (DM), belong to medical material DM production technical field.
Background technology
Medical material DM is an intermediate of producing third generation cephalosporin class microbiotic Qusong, thiophene oxime.Generally not high with existing method synthetic DM purity, fusing point generally about 170～172 ℃, can only be used for thiofide, and can not DM further must be purified or improve synthetic DM synthesis technique as the raw material of synthetic medicine.Document (polymkeric substance and auxiliary agent, 2004,2:38) reported with benzene kind solvent highly industry DM, produce the method that to use DM, the DM fusing point that obtains can reach 181 ℃, basically meet the requirement of making active ester, but be to use benzene kind solvent still all can produce detrimentally affect surrounding environment to operator.The DM that produces content height, fusing point height, melting range weak point is the key that realizes pharmaceutical grade DM widespread use.
Summary of the invention
The object of the present invention is to provide a kind of is the method for oxidant production medical material DM with the hydrogen peroxide, and this procedure is simple, is easy to industrialization.Sodium sulfate in the water is recyclable, and water and Virahol can recycles, meets the environmental protection policy of country.
For achieving the above object, the present invention is realized by following technical proposals: a kind of is the method for oxidant production medical material DM with the hydrogen peroxide, it is characterized in that comprising following process:
1. the weight ratio of water and rubber accelerator M is in 1～15: the 1 adding reactor, adding and rubber accelerator M mol ratio are 1: 1～3 sodium hydroxide, the M sodium salt liquid that reaction generates joins in the stills for air blowing, (solvent is a water to add volume ratio with M sodium salt liquid again and be 1: 1～10 solvent, ethanol, methyl alcohol, Virahol, acetone, aniline, toluene etc.), under 40～70 ℃ condition, dropping sulfuric acid and hydrogen peroxide weight ratio are 1: 1～12 mixed oxidization agent solution in solution, flow velocity is 50～110ml/ minute, up to the PH of solution is to stop to drip blending oxidizing agent at 4～8 o'clock, suction filtration, washing, filter, the dry medical material DM product that gets, the yield of medical material DM reaches more than 95%.
The invention has the advantages that: the sodium sulfate in the water is recyclable, and water and Virahol can recycles, meets the environmental protection policy of country.The purity of medical material DM can reach 99%, fusing point is more than 178 ℃.
Embodiment
Example 1:
The weight ratio of water and rubber accelerator M is to add reactor at 1: 1, adding and rubber accelerator M mol ratio are 1: 1 sodium hydroxide, the M sodium salt liquid that reaction generates joins in the stills for air blowing, the volume ratio of adding and M sodium salt liquid is 1: 1 a solvent (solvent is a water) again, under the temperature of reaction of 40C, dropping sulfuric acid and hydrogen peroxide weight ratio are 1: 2 mixed oxidization agent solution in solution, flow velocity is 50ml/ minute, up to the PH of solution is to stop to drip blending oxidizing agent at 8 o'clock, suction filtration, washing, filter, the dry medical material DM product that gets, the yield of medical material DM reaches more than 94%.The invention has the advantages that: the sodium sulfate in the water is recyclable, and water and Virahol can recycles, meets the environmental protection policy of country.The purity of medical material DM can reach 99%, fusing point is more than 178 ℃.
Example 2:
The weight ratio of water and rubber accelerator M is to add reactor at 1: 1, adding and rubber accelerator M mol ratio are 1: 1.5 sodium hydroxide, the M sodium salt liquid that reaction generates joins in the stills for air blowing, the volume ratio of adding and M sodium salt liquid is 1: 2 a solvent (solvent is an ethanol) again, under 40 ℃ temperature of reaction, dropping sulfuric acid and hydrogen peroxide weight ratio are 1: 2 mixed oxidization agent solution in solution, flow velocity is 50/ minute, up to the PH of solution is to stop to drip blending oxidizing agent at 8 o'clock, suction filtration, washing, filter, the dry medical material DM product that gets, the yield of medical material DM reaches more than 95%.The invention has the advantages that: the sodium sulfate in the water is recyclable, and water and Virahol can recycles, meets the environmental protection policy of country.The purity of medical material DM can reach 99%, fusing point is more than 179 ℃.
Example 3:
The weight ratio of water and rubber accelerator M is in the 11 adding reactors, adding and rubber accelerator M mol ratio are 1: 1.2 sodium hydroxide, the M sodium salt liquid that reaction generates joins in the stills for air blowing, the volume ratio of adding and M sodium salt liquid is 1: 3 a solvent (solvent is an acetone) again, under 40 ℃ temperature of reaction, dropping sulfuric acid and hydrogen peroxide weight ratio are 1: 3 mixed oxidization agent solution in solution, flow velocity is 50/ minute, up to the PH of solution is to stop to drip blending oxidizing agent at 4 o'clock, suction filtration, washing, filter, the dry medical material DM product that gets, the yield of medical material DM reaches more than 95%.The invention has the advantages that: the sodium sulfate in the water is recyclable, and water and Virahol can recycles, meets the environmental protection policy of country.The purity of medical material DM can reach 99%, fusing point is more than 180 ℃.
Claims (1)
1. one kind is the method for oxidant production medical material DM with the hydrogen peroxide, it is characterized in that comprising following process: the weight ratio of water and rubber accelerator M is in 1～15: the 1 adding reactor, adding and rubber accelerator M mol ratio are 1: 1～3 sodium hydroxide, the M sodium salt liquid that reaction generates joins in the stills for air blowing, (solvent is a water to add volume ratio with M sodium salt liquid again and be 1: 1～10 solvent, ethanol, methyl alcohol, Virahol, acetone, aniline, toluene etc.), under 40～70 ℃ condition, dropping sulfuric acid and hydrogen peroxide weight ratio are 1: 1～12 mixed oxidization agent solution in solution, flow velocity is 50～110ml/ minute, up to the PH of solution is to stop to drip blending oxidizing agent at 4～8 o'clock, suction filtration, washing, filter, the dry medical material DM product that gets, the yield of medical material DM reaches more than 95%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101285556A CN101899019A (en) | 2010-03-22 | 2010-03-22 | Method for producing medical raw material DM by using oxydol as oxidant |
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| CN2010101285556A CN101899019A (en) | 2010-03-22 | 2010-03-22 | Method for producing medical raw material DM by using oxydol as oxidant |
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| CN101899019A true CN101899019A (en) | 2010-12-01 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030720A (en) * | 2010-12-08 | 2011-04-27 | 河南省开仑化工有限责任公司 | Novel process for producing rubber vulcanization accelerator DM |
| CN102775369A (en) * | 2012-08-28 | 2012-11-14 | 山东邹平开元化工石材有限公司 | Vulcanization accelerator DM production process |
| CN102838559A (en) * | 2012-09-25 | 2012-12-26 | 科迈化工股份有限公司 | Preparation method of rubber accelerator dibenzothiazyl disulfide |
| CN102863401A (en) * | 2012-09-17 | 2013-01-09 | 温州市嘉力化工有限公司 | Novel process for producing medical intermediate DM (dibenzothiazyl disulfide) |
| CN103193732A (en) * | 2013-04-25 | 2013-07-10 | 宝月（天津）环保工程有限公司 | Preparation method of rubber vulcanization accelerator DM |
| CN104230843A (en) * | 2014-08-29 | 2014-12-24 | 山东海迈新材料有限公司 | Process for sectional oxosynthesis of DM (dibenzothiazyl disulfide) |
| CN104262288A (en) * | 2014-09-15 | 2015-01-07 | 河南省开仑化工有限责任公司 | Production method of rubber vulcanization accelerator DM |
| CN107879995A (en) * | 2017-10-26 | 2018-04-06 | 淄博鑫泉医药技术服务有限公司 | The method that the M synthesis DM reclaimed in raffinate is synthesized using cefotaxime acid |
| CN108341790A (en) * | 2018-01-08 | 2018-07-31 | 浙江鸿浩科技有限公司 | A kind of method of photocatalysis organic synthesis accelerating agent |
| CN109810075A (en) * | 2019-03-03 | 2019-05-28 | 朝阳天铭工贸有限公司 | A kind of technique of isopropanol method purification DM |
| CN110746373A (en) * | 2019-12-06 | 2020-02-04 | 广东省生物医药技术研究所 | Method for preparing 2, 2' -dithiodibenzothiazole from crude pinosylvin sodium mother liquor and application thereof |
| CN110776477A (en) * | 2019-11-27 | 2020-02-11 | 山东省化工研究院 | Method for preparing DM by oxidizing M with hydrogen peroxide |
-
2010
- 2010-03-22 CN CN2010101285556A patent/CN101899019A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030720A (en) * | 2010-12-08 | 2011-04-27 | 河南省开仑化工有限责任公司 | Novel process for producing rubber vulcanization accelerator DM |
| CN102775369A (en) * | 2012-08-28 | 2012-11-14 | 山东邹平开元化工石材有限公司 | Vulcanization accelerator DM production process |
| CN102863401B (en) * | 2012-09-17 | 2014-10-29 | 温州市嘉力化工有限公司 | Novel process for producing medical intermediate DM (dibenzothiazyl disulfide) |
| CN102863401A (en) * | 2012-09-17 | 2013-01-09 | 温州市嘉力化工有限公司 | Novel process for producing medical intermediate DM (dibenzothiazyl disulfide) |
| CN102838559A (en) * | 2012-09-25 | 2012-12-26 | 科迈化工股份有限公司 | Preparation method of rubber accelerator dibenzothiazyl disulfide |
| CN103193732B (en) * | 2013-04-25 | 2015-04-22 | 宝月（天津）环保工程有限公司 | Preparation method of rubber vulcanization accelerator DM |
| CN103193732A (en) * | 2013-04-25 | 2013-07-10 | 宝月（天津）环保工程有限公司 | Preparation method of rubber vulcanization accelerator DM |
| CN104230843A (en) * | 2014-08-29 | 2014-12-24 | 山东海迈新材料有限公司 | Process for sectional oxosynthesis of DM (dibenzothiazyl disulfide) |
| CN104230843B (en) * | 2014-08-29 | 2016-06-29 | 山东海迈新材料有限公司 | The technique of staged oxidation synthesis DM |
| CN104262288A (en) * | 2014-09-15 | 2015-01-07 | 河南省开仑化工有限责任公司 | Production method of rubber vulcanization accelerator DM |
| CN104262288B (en) * | 2014-09-15 | 2019-03-08 | 河南省开仑化工有限责任公司 | A kind of production method of rubber vulcanization accelerator DM |
| CN107879995A (en) * | 2017-10-26 | 2018-04-06 | 淄博鑫泉医药技术服务有限公司 | The method that the M synthesis DM reclaimed in raffinate is synthesized using cefotaxime acid |
| CN108341790A (en) * | 2018-01-08 | 2018-07-31 | 浙江鸿浩科技有限公司 | A kind of method of photocatalysis organic synthesis accelerating agent |
| CN108341790B (en) * | 2018-01-08 | 2021-12-17 | 浙江鸿浩科技有限公司 | Method for photocatalytic organic synthesis of promoter |
| CN109810075A (en) * | 2019-03-03 | 2019-05-28 | 朝阳天铭工贸有限公司 | A kind of technique of isopropanol method purification DM |
| CN110776477A (en) * | 2019-11-27 | 2020-02-11 | 山东省化工研究院 | Method for preparing DM by oxidizing M with hydrogen peroxide |
| CN110776477B (en) * | 2019-11-27 | 2023-03-10 | 山东省化工研究院 | Method for preparing DM by oxidizing M with hydrogen peroxide |
| CN110746373A (en) * | 2019-12-06 | 2020-02-04 | 广东省生物医药技术研究所 | Method for preparing 2, 2' -dithiodibenzothiazole from crude pinosylvin sodium mother liquor and application thereof |
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Application publication date: 20101201 |