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Preparation method of terbutaline sulfate
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A technology of terbutaline sulfate and acid binding agent, which is applied in the field of preparation of terbutaline sulfate, can solve the problems of expensive raw materials, long reaction steps, complicated operations, etc. Mild conditions, long solution steps and low yield
Active Publication Date: 2020-04-03
ZHEJIANG PHARMA COLLEGE
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[0009] Purpose of the invention: In order to solve the technical problems in the existing synthesis process of terbutaline sulfate, such as expensive and difficult to obtain raw materials, use of high-risk and highly toxic reagents, long reaction steps, low yield, cumbersome operation and other technical problems, a terbutaline sulfate is provided Forest preparation method
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Embodiment 1
[0033] A preparation method of terbutaline sulfate, specifically comprising:
[0034] (1) Preparation of 3,5-dibenzyloxyacetophenone
[0035] At room temperature, 100.0g (657.25mmol) of 3,5-dihydroxyacetophenone, 227.1g (1.64mol) of anhydrouspotassiumcarbonate, 1L of acetone and 174.7g (1.38mol) of benzyl chloride were successively added to the reaction vessel. , Reacted at 50°C for 6h. The reaction solution was cooled to room temperature, filtered with suction, the filter cake was washed with acetone (2×100mL), the combined filtrate was evaporated under reduced pressure to remove the acetone, and the residue was recrystallized with methanol to obtain an off-white solid, namely 3,5-dibenzyloxybenzene Ethanone 175.0g, yield 80%.
[0048] A preparation method of terbutaline sulfate, specifically comprising:
[0049] (1) Preparation of 3,5-dibenzyloxyacetophenone
[0050] At room temperature, 150.0g (985.88mmol) of 3,5-dihydroxyacetophenone, 313.4g (2.27mol) of anhydrouspotassiumcarbonate, 1L of acetone and 262.1g (2.07mol) of benzyl chloride were successively added to the reaction vessel, and the addition was completed. , React at 60°C for 4h. The reaction solution was cooled to room temperature, filtered with suction, the filter cake was washed with acetone (2×100mL), the combined filtrate was evaporated under reduced pressure to remove the acetone, and the residue was recrystallized with methanol to obtain an off-white solid, namely 3,5-dibenzyloxybenzene Ethanone 268.7g, yield 82%.
[0052] (2) Preparation of 3,5-dibenzyloxyacetophenone aldehyde
[0053] At room tempera...
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Abstract
The invention discloses a preparation method of terbutalinesulfate. The method comprises the steps: taking 3,5-dihydroxyacetophenone as an initial raw material, firstly, carrying out benzyl protection to obtain 3,4-dibenzyloxyacetophenone, carrying out copperbromide bromination and DMSO oxidation on 3,5-dibenzyloxyacetophenone to obtain 3,5-dibenzyloxyacetophenone aldehyde, carrying out reductive amination on 3,5-dibenzyloxyacetophenone aldehyde and tert-butylamine to generate 1-[3,5-di(benzyloxy)phenyl]-2-(tert-butylamino)ethanol, and finally carrying out hydrogenation debenzylation and sulfuric acid salification, to obtain terbutalinesulfate. Compared with the prior art, the method has the advantages that the used raw materials and auxiliary materials are cheap and easily available, the use of high-risk and highly-toxic reagents is avoided, high-temperature and high-pressure reaction is avoided, the operation is simple and convenient, the reaction conditions are mild, and the defects of long steps, low yield, potential safety hazards and the like in the prior art are overcome.
Description
technical field [0001] The invention relates to a preparation method of terbutalinesulfate, belonging to the technical field of terbutaline sulfate synthesis. Background technique [0002] TerbutalineSulfate, also known as hydroxyalbutaline and terbutaline, is an adrenergicagonist that selectively stimulates β2 receptors to relax bronchial smooth muscle and inhibit endogenous spasm-causing substances release and endogenous mediator-induced edema, and improve bronchial mucociliary epithelial clearance. It was first developed by AstraZeneca Pharmaceutical Co., Ltd., and it was produced and marketed abroad in 1988. Clinically, it is mainly used for the treatment of bronchospasm in bronchial asthma, asthmatic bronchitis and chronic obstructive pulmonary disease. [0003] At present, many synthetic processes for terbutaline sulfate have been reported at home and abroad, but there are certain technical problems, such as long process routes, expensive raw materials, and highly...
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