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Separation method and application of naphthol derivatives

A technology of naphthol derivatives and separation methods, which is applied in the field of separation of naphthol derivatives, can solve problems such as the inability to separate 1-isopropylamino-3-(2-naphthyloxy)-2-propanol, and achieve Good separation and simple operation

Active Publication Date: 2022-03-15
WUHAN CONFORM PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to overcome the problem that the prior art cannot carry out good separation of 1-isopropylamino-3-(2-naphthyloxy)-2-propanol and propranolol hydrochloride, thereby providing A kind of separation method and application of naphthol derivatives

Method used

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  • Separation method and application of naphthol derivatives
  • Separation method and application of naphthol derivatives
  • Separation method and application of naphthol derivatives

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Instruments: Agilent 1260 high performance liquid chromatography, electronic analytical balance, pH meter

[0060] The ratio of the mobile phase is a mixture of acetonitrile-water-sulfuric acid (50:50:0.1) (take 1.6g of sodium lauryl sulfate and 0.31g of tetrabutylammonium dihydrogen phosphate and dissolve it in 1000ml of the mixture, use 2mol / L sodium hydroxide solution adjusts the pH value to 3.3);

[0061] The chromatographic column is Agilent SB C18 (250mm×4.6mm×5μm);

[0062] The flow rate is 1.2ml / min;

[0063] The detection wavelength is 230nm;

[0064] Column temperature 40°C;

[0065] Accurately weigh 3-(1-naphthyloxy)-1,2-propanediol, 1-isopropylamino-3-(2-naphthyloxy)-2-propanol, 1-naphthylglycidyl ether , 1,2-di-isopropylamino-3-(1-naphthyloxy)-2-propanol, 1,3-di-(1-naphthyloxy)propan-2-ol and 3,3'- An appropriate amount of (isopropylamino)-di-(1-naphthyloxy)propan-2-ol, the mobile phase is diluted to contain 3-(1-naphthyloxy)-1,2-propanediol, 1- Isop...

Embodiment 2

[0108] All the other operations are as in Example 1, only the mobile phase is changed to the mixed solution of acetonitrile-water-sulfuric acid (51:49:0.1) (sodium lauryl sulfate 1.6g and tetrabutylammonium dihydrogen phosphate 0.31g are dissolved in In the 1000ml mixed solution, adjust the pH value to 3.3 with 2mol / L sodium hydroxide solution), and the sample adopts the resolution solution and the test solution.

[0109] See the attached chromatogram for details Figure 9 and 10 .

[0110] The analytical detection result of resolution solution is as shown in table 9:

[0111] Table 9

[0112]

[0113] Among them, the peak numbers are assigned as follows:

[0114] Peak number 1 is 3-(1-naphthyloxy)-1,2-propanediol;

[0115] Peak number 2 is 1-isopropylamino-3-(2-naphthyloxy)-2-propanol;

[0116] Peak No. 3 is propranolol hydrochloride;

[0117] Peak number 4 is 1-naphthyl glycidyl ether;

[0118] Peak number 5 is 1,2-di-isopropylamino-3-(1-naphthyloxy)-2-propanol; ...

Embodiment 3

[0130] All the other operations are as in Example 1, only the mobile phase is changed to the mixed solution of acetonitrile-water-sulfuric acid (49:51:0.1) (sodium lauryl sulfate 1.6g and tetrabutylammonium dihydrogen phosphate 0.31g are dissolved in In the 1000ml mixed solution, adjust the pH value to 3.3 with 2mol / L sodium hydroxide solution), and the sample adopts the resolution solution and the test solution.

[0131] See the attached chromatogram for details Figure 11 and 12 .

[0132] The analytical detection result of resolution solution is as shown in table 11:

[0133] Table 11

[0134]

[0135]

[0136] Among them, the peak numbers are assigned as follows:

[0137] Peak number 1 is 3-(1-naphthyloxy)-1,2-propanediol;

[0138] Peak number 2 is 1-isopropylamino-3-(2-naphthyloxy)-2-propanol;

[0139] Peak No. 3 is propranolol hydrochloride;

[0140] Peak number 4 is 1-naphthyl glycidyl ether;

[0141] Peak number 5 is 1,2-di-isopropylamino-3-(1-naphthyloxy...

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Abstract

The invention discloses a separation method and application of naphthol derivatives. The present invention separates 1-isopropylamino-3-(2-naphthyloxy)-2-propanol and propranolol hydrochloride through the separation method of high-efficiency liquid phase; the method is simple to operate and has good separation degree. It can also take into account the separation of other impurities in propranolol hydrochloride, and is suitable for the separation and detection of various known or unknown impurities produced under synthetic conditions.

Description

technical field [0001] The invention relates to a separation method and application of naphthol derivatives. Background technique [0002] Propranolol hydrochloride, as shown in the following formula, has a chemical name of 1-isopropylamino-3-(l-naphthyloxy)-2-propanol hydrochloride, which is a non-selective beta-receptor blocker, Block myocardial β receptors, and have antagonistic effects on both β1 and β2 receptors. It is clinically used to treat diseases such as hypertension, angina pectoris and arrhythmia, and the drug effect is good. [0003] [0004] The synthetic technique of propranolol hydrochloride mainly takes 1-naphthol and epichlorohydrin as starting raw materials at present, through intermediate 1-naphthyl glycidyl ether, and then through intermediate 1-isopropylamino-3 -(1-naphthyloxy)-2-propanol reacts with hydrochloric acid to generate propranolol hydrochloride. [0005] According to the 1-naphthol national standard (GBT 25782-2010), it can be seen tha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 周小顺牟东升余雪峰李进贺容丽别彤
Owner WUHAN CONFORM PHARMA CO LTD
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