CN105693525A - 2-dimethylaminoethyl chloride hydrochloride synthesis technology - Google Patents
2-dimethylaminoethyl chloride hydrochloride synthesis technology Download PDFInfo
- Publication number
- CN105693525A CN105693525A CN201410699964.XA CN201410699964A CN105693525A CN 105693525 A CN105693525 A CN 105693525A CN 201410699964 A CN201410699964 A CN 201410699964A CN 105693525 A CN105693525 A CN 105693525A
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- CN
- China
- Prior art keywords
- reaction
- product
- synthesis technology
- chloride hydrochloride
- hydrochloride synthesis
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- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 15
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 14
- 238000005516 engineering process Methods 0.000 title abstract description 5
- LQLJZSJKRYTKTP-UHFFFAOYSA-N 2-dimethylaminoethyl chloride hydrochloride Chemical compound Cl.CN(C)CCCl LQLJZSJKRYTKTP-UHFFFAOYSA-N 0.000 title abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005457 ice water Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 4
- 229960002887 deanol Drugs 0.000 claims abstract description 4
- 239000012972 dimethylethanolamine Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 18
- WQMAANNAZKNUDL-UHFFFAOYSA-N 2-dimethylaminoethyl chloride Chemical compound CN(C)CCCl WQMAANNAZKNUDL-UHFFFAOYSA-N 0.000 claims description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 abstract 2
- 239000007795 chemical reaction product Substances 0.000 abstract 2
- 239000002699 waste material Substances 0.000 abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 abstract 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract 1
- 229910017053 inorganic salt Inorganic materials 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000012452 mother liquor Substances 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 238000001953 recrystallisation Methods 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000007867 post-reaction treatment Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a 2-dimethylaminoethyl chloride hydrochloride synthesis technology. The technology comprises that dimethylethanolamine as a raw material and thionyl chloride directly undergo a chlorination reaction in an ice water bath under control of a temperature in a range of 8-18 DEG C, anhydrous ethanol is added into the reaction product, the mixture undergoes a reflux reaction for 2h, and the reaction product is filtered and dried so that a finished product is obtained. The 2-dimethylaminoethyl chloride hydrochloride synthesis technology has the advantages that 1, the product is free of recrystallization and has a high yield, good quality and a low cost, 2, reaction conditions are mild and are convenient for operation, 3, product purity is high and inorganic salt content is less than 0.5%, and 4, three wastes are reduced, hydrogen chloride and sulfur dioxide gas in the reaction are absorbed and the mother liquor subjected to pumping filtration is free of after treatment and is subjected to waste liquid delegation treatment so that environmental protection is promoted.
Description
Technical field
The invention belongs to technical field of chemical synthesis, be specifically related to the synthesis technique of a kind of 2-dimethylamino ethyl chloride hydrochlorate。
Background technology
The processes such as the synthesis technique of 2-dimethylamino ethyl chloride hydrochlorate at least includes drying, ice-water bath, filtration reaction。In current 2-dimethylamino ethyl chloride hydrochlorate building-up process method, technological process is not easy to implement, the 2-dimethylamino ethyl chloride hydrochlorate finished product purity generated is low, reaction residual cannot be recycled, manufacturing process is complicated, production efficiency is low and cost high, is not suitable for large-scale production。
Summary of the invention
For the above-mentioned technical problem overcoming prior art to exist, it is an object of the invention to, the synthesis technique of a kind of 2-dimethylamino ethyl chloride hydrochlorate is provided, the present invention not only manufacturing process is simple, improve work efficiency, and the 2-dimethylamino ethyl chloride hydrochlorate product purity generated is greatly, is suitable for industrialized production。
The synthesis technique of 2-dimethylamino ethyl chloride hydrochlorate provided by the invention, comprises the following steps:
(1) with dimethylethanolamine for raw material, ice-water bath condition controls temperature 8～18 DEG C and is made directly chlorination reaction with thionyl chloride；
(2) dehydrated alcohol back flow reaction is added 2 hours；
(3) filter, dry to obtain finished product。
The synthesis technique of 2-dimethylamino ethyl chloride hydrochlorate provided by the invention, it has the beneficial effects that, overcoming prior art, to prepare operation in 2-dimethylamino ethyl chloride hydrochloride process process more, and the problem that workload is big improves work efficiency；Improve the conversion per pass of reactant and the productivity of product。
Detailed description of the invention
Below in conjunction with an embodiment, the synthesis technique of 2-dimethylamino ethyl chloride hydrochlorate provided by the invention is described in detail。
Embodiment
The synthesis technique of the 2-dimethylamino ethyl chloride hydrochlorate of the present embodiment, comprises the following steps:
(1) with dimethylethanolamine for raw material, ice-water bath condition controls temperature 12 DEG C and is made directly chlorination reaction with thionyl chloride；
(2) dehydrated alcohol back flow reaction is added 2 hours；
(3) filter, dry to obtain finished product。
The synthesis technique of 2-dimethylamino ethyl chloride hydrochlorate, it is not necessary to loaded down with trivial details post-reaction treatment, substantially increases properties of product, and it is environmentally friendly pollution-free, technological process is easy to implement, and production cost is low, synthesis yield is high, better achieves the industrialized production of product。
Claims (1)
1. the synthesis technique of a 2-dimethylamino ethyl chloride hydrochlorate, it is characterised in that: said method comprising the steps of:
(1) with dimethylethanolamine for raw material, ice-water bath condition controls temperature 8～18 DEG C and is made directly chlorination reaction with thionyl chloride；
(2) dehydrated alcohol back flow reaction is added 2 hours；
(3) filter, dry to obtain finished product。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410699964.XA CN105693525A (en) | 2014-11-28 | 2014-11-28 | 2-dimethylaminoethyl chloride hydrochloride synthesis technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410699964.XA CN105693525A (en) | 2014-11-28 | 2014-11-28 | 2-dimethylaminoethyl chloride hydrochloride synthesis technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105693525A true CN105693525A (en) | 2016-06-22 |
Family
ID=56294584
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410699964.XA Pending CN105693525A (en) | 2014-11-28 | 2014-11-28 | 2-dimethylaminoethyl chloride hydrochloride synthesis technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105693525A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445847A (en) * | 2017-07-31 | 2017-12-08 | 昆山三友医药原料有限公司 | The synthesis technique of 2 dimethylamino chloroethanes hydrochlorides |
-
2014
- 2014-11-28 CN CN201410699964.XA patent/CN105693525A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445847A (en) * | 2017-07-31 | 2017-12-08 | 昆山三友医药原料有限公司 | The synthesis technique of 2 dimethylamino chloroethanes hydrochlorides |
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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: 20160622 |
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| WD01 | Invention patent application deemed withdrawn after publication |