CN109912476A - A kind of production technology of isopropylamino sulfonic acid chloride - Google Patents
A kind of production technology of isopropylamino sulfonic acid chloride Download PDFInfo
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- CN109912476A CN109912476A CN201910239955.5A CN201910239955A CN109912476A CN 109912476 A CN109912476 A CN 109912476A CN 201910239955 A CN201910239955 A CN 201910239955A CN 109912476 A CN109912476 A CN 109912476A
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- isopropylamino
- sulfonic acid
- acid chloride
- production technology
- chloride according
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Abstract
The invention discloses a kind of production technologies of isopropylamino sulfonic acid chloride, in dry conditions, isopropylamine hydrochloride is added in solvent, chlorosulfuric acid is slowly added dropwise, the temperature that chlorosulfuric acid is added dropwise is 10-20 DEG C, the solvent is acetonitrile, drip off rear temperature reaction for a period of time, reaction temperature is 20-70 DEG C, is cooled down after reaction, and front-end volatiles are obtained by air-distillation, then obtain product isopropylamino sulfonic acid chloride through high-vacuum pump rectification under vacuum.The purity of product isopropylamino sulfonic acid chloride of the invention reaches 98% or more, and highest molar yield is close to 80%.
Description
Technical field
The invention belongs to chemical production fields, and in particular to a kind of production technology of isopropylamino sulfonic acid chloride.
Background technique
The preparation of usual isopropylamino sulfonic acid chloride is first to act on isopropylamine and hydrochloric acid, generates isopropylamine hydrochloride, is dehydrated,
Then 90%~95% or more isopropyl ammonia is made with sulfonic acid chloride back flow reaction in acetonitrile solvent in isopropylamine hydrochloride by yield
Base sulfonic acid chloride.
Summary of the invention
Goal of the invention: in order to solve the deficiencies in the prior art, the present invention provides a kind of productions of isopropylamino sulfonic acid chloride
Technique.
Technical solution: isopropylamine hydrochloride is added in dry conditions for a kind of production technology of isopropylamino sulfonic acid chloride
In solvent, chlorosulfuric acid is slowly added dropwise, the temperature that chlorosulfuric acid is added dropwise is 10-20 DEG C, and the solvent is acetonitrile, is heated up after dripping off anti-
Should for a period of time, reaction temperature is 20-70 DEG C, is cooled down after reaction, and obtain front-end volatiles by air-distillation, then through high vacuum
Pump rectification under vacuum obtains product isopropylamino sulfonic acid chloride.
As optimization: the molar ratio of the isopropylamine hydrochloride and chlorosulfuric acid is 1:1-6.
As optimization: the molar ratio of the isopropylamine hydrochloride and chlorosulfuric acid is 1:3.
As optimization: the molar ratio of the isopropylamine hydrochloride and acetonitrile is 1:3-10.
As optimization: the molar ratio of the isopropylamine hydrochloride and acetonitrile is 1:6.
As optimization: the reaction temperature of temperature reaction is 50 DEG C.
As optimization: the air-distillation temperature is 80-90 DEG C.
As optimization: when rectification under vacuum, vacuum degree collects 74-75 DEG C of product at 19mmHg.
As optimization: tail gas HCl is absorbed by 1 grade of falling liquid film water and 1 grade of alkali spray-absorption processing.
The utility model has the advantages that the purity of product isopropylamino sulfonic acid chloride of the invention reaches 98% or more, highest molar yield is connect
Nearly 80%.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, so that the technology of this field
Personnel can better understand advantages and features of the invention, to make apparent boundary to protection scope of the present invention
It is fixed.Embodiment described in the invention is only a part of the embodiment of the present invention, instead of all the embodiments, based on the present invention
In embodiment, those of ordinary skill in the art's every other implementation obtained without making creative work
Example, shall fall within the protection scope of the present invention.
Specific embodiment 1
A kind of production technology of isopropylamino sulfonic acid chloride isopropylamine hydrochloride is added in solvent, slowly in dry conditions
Slow that chlorosulfuric acid is added dropwise, the temperature that chlorosulfuric acid is added dropwise is 10 DEG C, and the solvent is acetonitrile, drips off rear temperature reaction for a period of time,
Reaction temperature is 20 DEG C；Cool down after reaction, and obtains front-end volatiles by air-distillation, then must produce through high-vacuum pump rectification under vacuum
Product isopropylamino sulfonic acid chloride.
In the present embodiment, the molar ratio of the isopropylamine hydrochloride and chlorosulfuric acid is 1:1.The isopropylamine hydrochloride
Molar ratio with acetonitrile is 1:3.The air-distillation temperature is 80 DEG C.When rectification under vacuum, vacuum degree is collected at 19mmHg
74 DEG C of product.Tail gas HCl is absorbed by 1 grade of falling liquid film water and 1 grade of alkali spray-absorption processing.
Specific embodiment 2
A kind of production technology of isopropylamino sulfonic acid chloride isopropylamine hydrochloride is added in solvent, slowly in dry conditions
Slow that chlorosulfuric acid is added dropwise, the temperature that chlorosulfuric acid is added dropwise is 20 DEG C, and the solvent is acetonitrile, drips off rear temperature reaction for a period of time,
Reaction temperature is 70 DEG C；Cool down after reaction, and obtains front-end volatiles by air-distillation, then must produce through high-vacuum pump rectification under vacuum
Product isopropylamino sulfonic acid chloride.
In the present embodiment, the molar ratio of the isopropylamine hydrochloride and chlorosulfuric acid is 1:6.The isopropylamine hydrochloride
Molar ratio with acetonitrile is 1:10.The air-distillation temperature is 90 DEG C.When rectification under vacuum, vacuum degree is received at 19mmHg
The product of 75 DEG C of collection.Tail gas HCl is absorbed by 1 grade of falling liquid film water and 1 grade of alkali spray-absorption processing.
Specific embodiment 3
A kind of production technology of isopropylamino sulfonic acid chloride isopropylamine hydrochloride is added in solvent, slowly in dry conditions
Slow that chlorosulfuric acid is added dropwise, the temperature that chlorosulfuric acid is added dropwise is 14 DEG C, and the solvent is acetonitrile, drips off rear temperature reaction for a period of time,
Reaction temperature is 50 DEG C；Cool down after reaction, and obtains front-end volatiles by air-distillation, then must produce through high-vacuum pump rectification under vacuum
Product isopropylamino sulfonic acid chloride.
In the present embodiment, the molar ratio of the isopropylamine hydrochloride and chlorosulfuric acid is 1:3.The isopropylamine hydrochloride
Molar ratio with acetonitrile is 1:6.The air-distillation temperature is 84 DEG C.When rectification under vacuum, vacuum degree is collected at 19mmHg
74.5 DEG C of product.Tail gas HCl is absorbed by 1 grade of falling liquid film water and 1 grade of alkali spray-absorption processing.
The purity of product isopropylamino sulfonic acid chloride of the invention reaches 98% or more, and highest molar yield is close to 80%.
Claims (9)
1. a kind of production technology of isopropylamino sulfonic acid chloride, it is characterised in that: in dry conditions, isopropylamine hydrochloride is added
In solvent, chlorosulfuric acid is slowly added dropwise, the temperature that chlorosulfuric acid is added dropwise is 10-20 DEG C, and the solvent is acetonitrile, is heated up after dripping off anti-
Should for a period of time, reaction temperature is 20-70 DEG C, is cooled down after reaction, and obtain front-end volatiles by air-distillation, then through high vacuum
Pump rectification under vacuum obtains product isopropylamino sulfonic acid chloride.
2. the production technology of isopropylamino sulfonic acid chloride according to claim 1, it is characterised in that: the isopropylamine hydrochloric acid
The molar ratio of salt and chlorosulfuric acid is 1:1-6.
3. the production technology of isopropylamino sulfonic acid chloride according to claim 2, it is characterised in that: the isopropylamine hydrochloric acid
The molar ratio of salt and chlorosulfuric acid is 1:3.
4. the production technology of isopropylamino sulfonic acid chloride according to claim 1, it is characterised in that: the isopropylamine hydrochloric acid
The molar ratio of salt and acetonitrile is 1:3-10.
5. the production technology of isopropylamino sulfonic acid chloride according to claim 4, it is characterised in that: the isopropylamine hydrochloric acid
The molar ratio of salt and acetonitrile is 1:6.
6. the production technology of isopropylamino sulfonic acid chloride according to claim 1, it is characterised in that: the reaction temperature of temperature reaction
Degree is 50 DEG C.
7. the production technology of isopropylamino sulfonic acid chloride according to claim 1, it is characterised in that: the air-distillation temperature
Degree is 80-90 DEG C.
8. the production technology of isopropylamino sulfonic acid chloride according to claim 1, it is characterised in that: when rectification under vacuum, vacuum
Degree collects 74-75 DEG C of product at 19mmHg.
9. the production technology of isopropylamino sulfonic acid chloride according to claim 1, it is characterised in that: tail gas HCl is by 1 grade of drop
Film water absorbs and 1 grade of alkali spray-absorption processing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910239955.5A CN109912476A (en) | 2019-03-27 | 2019-03-27 | A kind of production technology of isopropylamino sulfonic acid chloride |
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| CN201910239955.5A CN109912476A (en) | 2019-03-27 | 2019-03-27 | A kind of production technology of isopropylamino sulfonic acid chloride |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2245331A1 (en) * | 1997-08-22 | 1999-02-22 | John Fairhurst | Pharmaceutical compounds |
| CN101730692A (en) * | 2007-03-15 | 2010-06-09 | 先灵公司 | Pyridazinone derivatives useful as glucan synthase inhibitors |
| CN107176917A (en) * | 2017-05-11 | 2017-09-19 | 蚌埠中实化学技术有限公司 | A kind of method for preparing dimethylamino sulfonic acid chloride |
-
2019
- 2019-03-27 CN CN201910239955.5A patent/CN109912476A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2245331A1 (en) * | 1997-08-22 | 1999-02-22 | John Fairhurst | Pharmaceutical compounds |
| CN101730692A (en) * | 2007-03-15 | 2010-06-09 | 先灵公司 | Pyridazinone derivatives useful as glucan synthase inhibitors |
| CN107176917A (en) * | 2017-05-11 | 2017-09-19 | 蚌埠中实化学技术有限公司 | A kind of method for preparing dimethylamino sulfonic acid chloride |
Non-Patent Citations (2)
| Title |
|---|
| 宋小平等: "《精细化工品实用生产技术手册 农药制造技术》", 30 April 2001, 北京：科学技术文献出版社 * |
| 胡汉兴等: "异丙胺基磺酰氯的合成方法", 《湖南化工》 * |
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Address after: 226000 Nantong Qidong Economic Development Zone Jiangsu fine chemical industry concentrated area Applicant after: Nantong baokai Pharmaceutical Co., Ltd Address before: 226000 Nantong Qidong Economic Development Zone Jiangsu fine chemical industry concentrated area Applicant before: Nantong Baokai Chemical Co.,Ltd. |
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Application publication date: 20190621 |