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A kind of dobutamine hydrochloride decolorization process

A dobutamine hydrochloride, process technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of unsatisfactory decolorization effect, quality not meeting the requirements of pharmacopoeia, and increased impurities

Inactive Publication Date: 2018-03-13
HEZE CITY FANGMING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the dobutamine hydrochloride molecule contains multiple phenolic hydroxyl groups that are easily oxidized, if the commonly used activated carbon decolorization method is used, the impurities will increase, the decolorization effect is not ideal, and the quality after decolorization cannot meet the requirements of the Pharmacopoeia.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 150ml of purified water into the reaction bottle, then add 0.30g of sodium bisulfite, 15g of dobutamine hydrochloride (light yellow in appearance, HPLC purity ≥ 99.5%, simple complex ≤ 0.1%), fill with nitrogen for 5 Then heat up to 90-100°C to dissolve, add 1.5g of activated carbon, keep warm for 60 minutes for decolorization, filter out the activated carbon by hot filtration, add 15g of concentrated hydrochloric acid to the filtrate, slowly cool down to 20°C for 6 hours, keep for 2 hours, and precipitate crystals. Filtrate and dry to obtain 12.7 g of dobutamine hydrochloride, which is white powder in appearance, HPLC purity ≥ 99.5%, single impurity ≤ 0.1%, yield 84.6%.

Embodiment 2

[0014] Add 150ml of purified water into the reaction bottle, then add 0.15g of sodium metabisulfite, 20g of dobutamine hydrochloride (light yellow in appearance, HPLC purity ≥ 99.5%, simple complex ≤ 0.1%), fill with nitrogen for 5 times, Then heat up to 90-100°C to dissolve, add 0.75g of activated carbon, keep warm for 60 minutes to decolorize, filter out the activated carbon by hot filtration, add 15g of concentrated hydrochloric acid to the filtrate, slowly cool down to 20°C for 6 hours, keep for 2 hours, precipitate crystals, filter out Dried to obtain 18.1 g of dobutamine hydrochloride, the appearance of a white powder, HPLC purity ≥ 99.5%, simplex ≤ 0.1%, yield 90.5%.

Embodiment 3

[0016] Add 150ml of purified water into the reaction bottle, then add 0.30g of sodium metabisulfite, 20g of dobutamine hydrochloride (light yellow in appearance, HPLC purity ≥ 99.5%, simple heterogeneity ≤ 0.1%), fill with nitrogen for 5 times, Then heat up to 90-100°C to dissolve, add 0.6g of activated carbon, keep warm for 30 minutes to decolorize, filter out the activated carbon by hot filtration, add 10g of concentrated hydrochloric acid to the filtrate, slowly cool down to 20°C for 6 hours, keep for 2 hours, precipitate crystals, filter out Dried to obtain 16.4 g of dobutamine hydrochloride, the appearance of a white powder, HPLC purity ≥ 99.5%, simplex ≤ 0.1%, yield 80.2%.

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Abstract

The invention belongs to the technical field of pharmacy and discloses a dobutamine hydrochloride decoloration technology. The technology comprises putting an anti-oxidant and dobutamine hydrochloride to be decolored into purified water, carrying out heating dissolution in an inert gas protective atmosphere, carrying out decoloration through adding active carbon into the solution, filtering to remove the active carbon in the hot solution, feeding the filtrate into a crystallization kettle, adding hydrochloric acid into the crystallization kettle, slowly cooling the filtrate so that solids are precipitated and carrying out filtration and drying to obtain white or off-white dobutamine hydrochloride. The technology can effectively remove colored substances in dobutamine hydrochloride, effectively inhibit impurity increasing caused by easy oxidation of dobutamine hydrochloride at a high temperature and produce a stable and high quality dobutamine hydrochloride finished product. The technology has the characteristics of simple processes, good decoloration effects, high yield, low cost and industrial production feasibility.

Description

technical field [0001] The invention relates to a dobutamine hydrochloride decolorization process, which belongs to the technical field of pharmacy. Background technique [0002] Dobutamine hydrochloride, chemical name: 4-[2-[[1-methyl-3-(4-hydroxyphenyl)propyl]amino]ethyl]-1,2-benzenediol hydrochloride , the English name Dobutamine Hydrochloride, the molecular formula is C18H23NO3·HCl, is a homologue of dopamine, a selective cardiac β1-receptor stimulant, and is clinically used to treat heart failure and myocardial infarction caused by organic heart disease with decreased myocardial contractility. Cardiogenic shock and postoperative hypotension. [0003] In the original synthesis technology, the preparation method of dobutamine hydrochloride is (US5073648A, WO2008047382): 3,4-dimethoxyphenethylamine is used as raw material, and p-methoxybutyrophenone is reacted with p-toluenesulfonic acid Down condensation into imine, and then use palladium charcoal catalytic hydrogenatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/10C07C215/54
CPCC07C213/10C07C215/54
Inventor 朱文祥段海梅葛丰伟
Owner HEZE CITY FANGMING PHARMA
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