- Preparation method of arotinolol hydrochloride
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The invention provides a preparation method of arotinolol hydrochloride, which comprises the following steps of: reacting a compound shown as a structural formula VIII with absolute methanol in the presence of concentrated sulfuric acid to obtain a compou
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- Preparation method of arotinolol hydrochloride
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The invention relates to the technical field of medicines, particularly provides a preparation method of arotinolol hydrochloride, and relates to the technical field of medicines. The preparation method of the arotinolol hydrochloride, provided by the invention, comprises the following steps: (1) enabling tetrahydrofuran, 2-formamide-5-(2-sulfydryl-1, 3-thiazole-4-yl)-thiophene, water, sodium bicarbonate and epoxy chloropropane to react to generate an intermediate product C181101170-I03; (2) carrying out a reaction on absolute ethyl alcohol, C181101170-I03 and tert-butylamine, so as to obtain an intermediate product C181101170-I02; (3) subjecting methanol, ethyl acetate, C181101170-I02 and concentrated hydrochloric acid to a reaction, and obtaining an arotinolol hydrochloride crude product; and (4) treating the arotinolol hydrochloride crude product with DMSO and acetone to obtain arotinolol hydrochloride. The product arotinolol hydrochloride obtained by the method is high in yield, high in purity and small in impurity, the purity of the product can be well controlled, and the method is suitable for industrial production.
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Paragraph 0124; 0129-0133; 0138-0142; 0147-0150
(2021/07/09)
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- Preparation process for arotinolol hydrochloride with high purity
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The invention discloses a preparation process for arotinolol hydrochloride with high purity. The preparation process comprises the following steps: pouring an acid-binding agent into an alcohol-watercompounded solvent, adding a compound namely 5-(2-sulfhydryl-4-thiazole)-2-thiophenecarboxamide, then adding epichlorohydrin, carrying out a reaction at a room temperature, and carrying out filteringand drying so as to obtain an intermediate III; pouring tert-butylamine into anhydrous ethanol, adding the intermediate III, carrying out a micro-reflux reaction, carrying out concentration, adding purified water, carrying out dissolving under heating, carrying out cooling, adjusting the pH value of an obtained solution to be acidic, carrying out washing with an organic solvent, adding ethanol into an aqueous layer, carrying out dissolving under heating, and carrying out cooling crystallization, and carrying out filtering so as to obtain a crude product; and pouring the crude product into an alcohol-water compounded solvent, carrying out dissolving under heating, and carrying out cooling crystallization, filtering and drying so as to obtain the arotinolol hydrochloride with high purity. The preparation process provided by the invention can effectively remove impurities from arotinolol hydrochloride, can reach a purity of 99.95% or above, and has simple operation and high yield.
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Paragraph 0034; 0035; 0042; 0043; 0050; 0051
(2018/03/26)
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- A hydrochloric acid arotinolol the preparation process of the new method
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The invention belongs to the technical field of medicines and particularly relates to a simple and efficient method for preparing selective beta 1 adrenoceptor antagonists 5-[2-[[[3-(1,1-dimethylethyl)amino]-2-hydroxypropyl]thio]-4-thiazolyl]-2-thiophene carboxamide hydrochloride. The method comprises the following steps: firstly, reacting 5-(2-mercapto-4-thiazolyl)-2-thiophenecarboxamide and epoxy chloropropane in the presence of Lewis acid as a catalyst in an organic solvent, after the reaction is completed by the monitoring of TLC, filtering and carrying out pressure reduced concentration to dryness to obtain an intermediate; and secondly, reacting the intermediate and t-butylamine in an organic solvent, cooling to room temperature, adding hydrochloric acid to adjust the pH, carrying out reflux reaction, naturally cooling and crystallizing to obtain arotinolol hydrochloride.
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Paragraph 0035; 0036; 0037; 0038
(2017/08/26)
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