CN111362823A - Production method of labetalol hydrochloride - Google Patents
Production method of labetalol hydrochloride Download PDFInfo
- Publication number
- CN111362823A CN111362823A CN201811589120.4A CN201811589120A CN111362823A CN 111362823 A CN111362823 A CN 111362823A CN 201811589120 A CN201811589120 A CN 201811589120A CN 111362823 A CN111362823 A CN 111362823A
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- Prior art keywords
- reaction kettle
- solution
- labetalol hydrochloride
- centrifuging
- reaction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/12—Preparation of carboxylic acid amides by reactions not involving the formation of carboxamide groups
Abstract
The invention relates to a method for producing labetalol hydrochloride, which comprises the following steps: (1) proportioning an alkaline water solution; preparing a glacial acetic acid solution; (2) adding labetalol hydrochloride ketone into a reaction kettle, and adding the proportioned alkaline water solution until the components are dissolved; (3) controlling the temperature of the reaction kettle, adding excessive potassium borohydride into the reaction kettle while stirring the reaction kettle to participate in the reaction, and controlling the reaction time; (4) adding the prepared glacial acetic acid into a reaction kettle to neutralize redundant potassium borohydride and then centrifuging; (5) adding acetone or hydrochloric acid into the centrifuged solution to adjust ph =5, reacting for 3-4 hours, and centrifuging; (6) adding 3 times of purified water and 0.03 times of activated carbon into the centrifuged solution for hot melting and decoloring; (7) filtering, adding into a reaction kettle for crystallization, centrifuging and drying to obtain the labetalol hydrochloride. The invention is simple and practical, and convenient to operate; the process is low-temperature controllable, green and environment-friendly, and has high production efficiency and low production cost.
Description
Technical Field
The invention belongs to the field of pharmacy, and particularly relates to a production method of labetalol hydrochloride.
Background
Labetalol hydrochloride is used for various hypertensive emergencies, such as hypertensive crisis, pheochromocytoma crisis, preeclampsia, hypertensive encephalopathy, hypertension caused by extensive burns, hypertension accompanied with coronary artery diseases or acute myocardial infarction hypertension and postoperative hypertension, and can also be used for controlling blood pressure in anesthesia.
In the current market, the preparation method of labetalol hydrochloride has low efficiency, low principle utilization rate and easy environmental pollution.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a method for producing labetalol hydrochloride, which is environment-friendly, simple and practical and is convenient to operate.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a production method of labetalol hydrochloride comprises the following steps:
(1) proportioning 30-40% of alkaline water solution by mass percent; preparing a glacial acetic acid solution with the concentration of 35-45%;
(2) adding labetalol hydrochloride ketone into a reaction kettle, and adding the proportioned alkaline water solution until the components are dissolved;
(3) controlling the temperature of the reaction kettle to be 50-60 ℃, adding excessive potassium borohydride into the reaction kettle while stirring the reaction kettle to participate in the reaction, and controlling the reaction time to be 3-5 hours;
(4) adding the prepared glacial acetic acid into a reaction kettle to neutralize redundant potassium borohydride and then centrifuging;
(5) adding acetone or hydrochloric acid into the centrifuged solution to adjust ph =5, reacting for 3-4 hours, and centrifuging;
(6) adding 3 times of purified water and 0.03 times of activated carbon into the centrifuged solution for hot melting and decoloring;
(7) filtering, adding into a reaction kettle for crystallization, centrifuging and drying to obtain the labetalol hydrochloride.
The invention is further improved in that: in the step (1), the aqueous alkali solution is a potassium chloride solution.
The method has the technical advantages that:
1. compared with the prior art, the preparation method of the labetalol hydrochloride has simple and practical process and convenient operation;
2. the invention is carried out under low temperature control, and the process is green and environment-friendly;
3. the invention has high production efficiency, high utilization rate of raw materials and less waste.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1:
the embodiment relates to a method for producing labetalol hydrochloride, which comprises the following steps:
(1) according to the mass percentage, the mixture ratio concentration is 35 percent of potassium chloride solution; preparing a glacial acetic acid solution with the concentration of 40%;
(2) adding labetalol hydrochloride ketone into a reaction kettle, and adding the proportioned alkaline water solution until the components are dissolved;
(3) controlling the temperature of the reaction kettle to be 55 ℃, adding excessive potassium borohydride into the reaction kettle while stirring the reaction kettle to participate in the reaction, and controlling the reaction time to be 4 hours;
(4) adding the prepared glacial acetic acid into a reaction kettle to neutralize redundant potassium borohydride and then centrifuging;
(5) adding acetone or hydrochloric acid into the centrifuged solution to adjust ph =5, reacting for 3.5 hours, and centrifuging;
(6) adding 3 times of purified water and 0.03 times of activated carbon into the centrifuged solution for hot melting and decoloring;
(7) filtering, adding into a reaction kettle for crystallization, centrifuging and drying to obtain the labetalol hydrochloride.
Example 2:
the embodiment relates to a method for producing labetalol hydrochloride, which comprises the following steps:
(1) according to the mass percentage, the mixture ratio concentration is 30 percent of potassium chloride solution; preparing a glacial acetic acid solution with the concentration of 42%;
(2) adding labetalol hydrochloride ketone into a reaction kettle, and adding the proportioned alkaline water solution until the components are dissolved;
(3) controlling the temperature of the reaction kettle to be 60 ℃, adding excessive potassium borohydride into the reaction kettle while stirring the reaction kettle to participate in the reaction, and controlling the reaction time to be 3.8 hours;
(4) adding the prepared glacial acetic acid into a reaction kettle to neutralize redundant potassium borohydride and then centrifuging;
(5) adding acetone or hydrochloric acid into the centrifuged solution to adjust ph =5, reacting for 3 hours, and centrifuging;
(6) adding 3 times of purified water and 0.03 times of activated carbon into the centrifuged solution for hot melting and decoloring;
(7) filtering, adding into a reaction kettle for crystallization, centrifuging and drying to obtain the labetalol hydrochloride.
In this embodiment, the glacial acetic acid is food grade glacial acetic acid.
It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (2)
1. The production method of labetalol hydrochloride is characterized by comprising the following steps:
(1) proportioning 30-40% of alkaline water solution by mass percent; preparing a glacial acetic acid solution with the concentration of 35-45%;
(2) adding labetalol hydrochloride ketone into a reaction kettle, and adding the proportioned alkaline water solution until the components are dissolved;
(3) controlling the temperature of the reaction kettle to be 50-60 ℃, adding excessive potassium borohydride into the reaction kettle while stirring the reaction kettle to participate in the reaction, and controlling the reaction time to be 3-5 hours;
(4) adding the prepared glacial acetic acid into a reaction kettle to neutralize redundant potassium borohydride and then centrifuging;
(5) adding acetone or hydrochloric acid into the centrifuged solution to adjust ph =5, reacting for 3-4 hours, and centrifuging;
(6) adding 3 times of purified water and 0.03 times of activated carbon into the centrifuged solution for hot melting and decoloring;
(7) filtering, adding into a reaction kettle for crystallization, centrifuging and drying to obtain the labetalol hydrochloride.
2. The method for producing labetalol hydrochloride according to claim 1, wherein: in the step (1), the aqueous alkali solution is a potassium chloride solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811589120.4A CN111362823A (en) | 2018-12-25 | 2018-12-25 | Production method of labetalol hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811589120.4A CN111362823A (en) | 2018-12-25 | 2018-12-25 | Production method of labetalol hydrochloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111362823A true CN111362823A (en) | 2020-07-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811589120.4A Pending CN111362823A (en) | 2018-12-25 | 2018-12-25 | Production method of labetalol hydrochloride |
Country Status (1)
| Country | Link |
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| CN (1) | CN111362823A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225674A (en) * | 2020-10-28 | 2021-01-15 | 天津大学 | Labetalol hydrochloride crystal form compound and preparation method and application thereof |
| CN113698316A (en) * | 2021-09-03 | 2021-11-26 | 安徽美致诚药业有限公司 | Preparation method of labetalol hydrochloride |
-
2018
- 2018-12-25 CN CN201811589120.4A patent/CN111362823A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225674A (en) * | 2020-10-28 | 2021-01-15 | 天津大学 | Labetalol hydrochloride crystal form compound and preparation method and application thereof |
| CN112225674B (en) * | 2020-10-28 | 2021-12-03 | 天津大学 | Labetalol hydrochloride crystal form compound and preparation method and application thereof |
| CN113698316A (en) * | 2021-09-03 | 2021-11-26 | 安徽美致诚药业有限公司 | Preparation method of labetalol hydrochloride |
| CN113698316B (en) * | 2021-09-03 | 2022-04-19 | 安徽美致诚药业有限公司 | Preparation method of labetalol hydrochloride |
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Application publication date: 20200703 |
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| WD01 | Invention patent application deemed withdrawn after publication |