CN104744354A - Preparation method of octenidine - Google Patents
Preparation method of octenidine Download PDFInfo
- Publication number
- CN104744354A CN104744354A CN201310728582.0A CN201310728582A CN104744354A CN 104744354 A CN104744354 A CN 104744354A CN 201310728582 A CN201310728582 A CN 201310728582A CN 104744354 A CN104744354 A CN 104744354A
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- compound
- octenidine
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- preparation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/72—Nitrogen atoms
- C07D213/74—Amino or imino radicals substituted by hydrocarbon or substituted hydrocarbon radicals
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of octenidine, wherein the preparation method comprises the following specific steps: a, carrying out a reaction of pyridine and thionyl chloride, to obtain a compound (I), mixing phenol with the compound (I), carrying out a reaction at the temperature of 160 DEG C, adding octadecylamine hydrochloride, carrying out a reaction at the temperature of 220 DEG C, cooling, adding a 2 mol/L hydrochloric acid, distilling with water steam to remove phenol, then adding a 10% sodium hydroxide solution, alkalizing, cooling, filtering and collecting solids, dissolving with dilute hydrochloric acid, decoloring, adding a 10% sodium hydroxide solution, alkalizing, filtering and collecting solids, washing with water, drying, and thus obtaining a white crystalline compound (III); and b, carrying out a reaction of the compound (III) and decamethylene chloride at the temperature of 120 DEG C, cooling to about 100 DEG C, adding dimethylformamide, stirring and dissolving, naturally cooling, filtering and collecting solids, and thus obtaining the white crystalline octenidine. According to the preparation method of octenidine, the preparation process is simple, the yield is high and the quality is good.
Description
Technical field
The present invention relates to field prepared by medicine, especially a kind of preparation method of octenidine.
Background technology
Octenidine is the particular purification agent for skin, mucous membrane and wound for biocide.It has special role to adhesion and synthetic chemistry cellular component and has very high anti-microbial activity to whole cell, two octenidine dihydrochloride (octenidine) may be considered to a kind of biocide of uniqueness, by playing its activity in the acellular toxin synthesis of point of application.Therefore, octenidine can not be considered to a kind of typical sanitas, as chlorhexidine or BETADINE.Owing to being at present to produce in octenidine, preparation method is complicated, yields poorly, poor quality.
Summary of the invention
The technical problem to be solved in the present invention is: in order to overcome above-mentioned middle Problems existing, provide a kind of preparation method of octenidine.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of octenidine, concrete steps are as follows: a. pyridine and sulfur oxychloride reaction, compound (I) can be obtained, phenol and compound (I) mixing, 160 DEG C of reactions, add octylamine salt hydrochlorate, react at 220 DEG C, cooling, add people 2mol/L hydrochloric acid, wet distillation removing phenol, add 10% sodium hydroxide solution alkalization again, cooling, filter collection solid, with diluted hydrochloric acid dissolution, decolouring, add 10% sodium hydroxide solution alkalization, filter collection solid, washing, dry, obtain the compound (III) of white crystals, b. compound (III) and two chlorodecanes, react, are chilled to about 100 DEG C, add dimethyl formamide, stirring and dissolving, naturally cooling at 120 DEG C, and filter collection solid, obtains the octenidine of white crystals.
The invention has the beneficial effects as follows: the preparation method of described a kind of octenidine, its preparation process is simple, and output is high, quality better.
Embodiment
Be described in further detail in conjunction with the present invention now.
The preparation method of a kind of octenidine of the present invention, concrete steps are as follows: a. pyridine and sulfur oxychloride reaction, can obtain compound (I), phenol and compound (I) mixing, 160 DEG C of reactions, add octylamine salt hydrochlorate, react at 220 DEG C, cooling, add people 2mol/L hydrochloric acid, wet distillation removing phenol, then add 10% sodium hydroxide solution alkalization, cooling, filter collection solid, with diluted hydrochloric acid dissolution, decolouring, adds 10% sodium hydroxide solution alkalization, filter collection solid, washing, dry, obtain the compound (III) of white crystals; B. compound (III) and two chlorodecanes, react, are chilled to about 100 DEG C, add dimethyl formamide, stirring and dissolving, naturally cooling at 120 DEG C, and filter collection solid, obtains the octenidine of white crystals.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to right.
Claims (1)
1. the preparation method of an octenidine, it is characterized in that concrete steps are as follows: a. pyridine and sulfur oxychloride reaction, can obtain compound (I), phenol and compound (I) mixing, 160 DEG C of reactions, add octylamine salt hydrochlorate, react at 220 DEG C, cooling, add people 2mol/L hydrochloric acid, wet distillation removing phenol, then add 10% sodium hydroxide solution alkalization, cooling, filter collection solid, with diluted hydrochloric acid dissolution, decolouring, adds 10% sodium hydroxide solution alkalization, filter collection solid, washing, dry, obtain the compound (III) of white crystals; B. compound (III) and two chlorodecanes, react, are chilled to about 100 DEG C, add dimethyl formamide, stirring and dissolving, naturally cooling at 120 DEG C, and filter collection solid, obtains the octenidine of white crystals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310728582.0A CN104744354A (en) | 2013-12-26 | 2013-12-26 | Preparation method of octenidine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310728582.0A CN104744354A (en) | 2013-12-26 | 2013-12-26 | Preparation method of octenidine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104744354A true CN104744354A (en) | 2015-07-01 |
Family
ID=53584706
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310728582.0A Pending CN104744354A (en) | 2013-12-26 | 2013-12-26 | Preparation method of octenidine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104744354A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111051285A (en) * | 2017-08-21 | 2020-04-21 | 迪氏曼卡博金艾美斯有限公司 | Octenidine-based compounds |
| CN114989076A (en) * | 2022-06-07 | 2022-09-02 | 八叶草健康产业研究院(厦门)有限公司 | Preparation method of octenidine base |
-
2013
- 2013-12-26 CN CN201310728582.0A patent/CN104744354A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111051285A (en) * | 2017-08-21 | 2020-04-21 | 迪氏曼卡博金艾美斯有限公司 | Octenidine-based compounds |
| CN114989076A (en) * | 2022-06-07 | 2022-09-02 | 八叶草健康产业研究院(厦门)有限公司 | Preparation method of octenidine base |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150701 |
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| WD01 | Invention patent application deemed withdrawn after publication |