Refining method of dorzalamide hydrochloride

A technology of dorzolamide hydrochloride and a purification method, which is applied to the purification field of dorzolamide hydrochloride, can solve the problems of easy occurrence of sticking walls, material loss, material viscosity and the like, and achieves less waste treatment, simple operation and high yield Effect

Inactive Publication Date: 2020-03-24
WUHAN WUYAO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When using dimethyl sulfoxide for refining, dimethyl sulfoxide is not easy to remove, which has a great impact on the purity of the product;

Method used

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  • Refining method of dorzalamide hydrochloride
  • Refining method of dorzalamide hydrochloride
  • Refining method of dorzalamide hydrochloride

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0035] Example 1

[0036] This embodiment provides a method for refining dorzolamide hydrochloride, which includes:

[0037] Dissolve the crude dorzolamide hydrochloride (100 g) in water (400 g) at 85-95°C. After filtration, ethanol (100 g) was added dropwise to this aqueous solution at 40 to 45°C. The temperature was gradually cooled to 0-5°C, stirred at this temperature for 2 to 4 hours, the filter cake obtained by filtration was washed with ethanol, and dried at 50°C for 8 hours. 91.2 g of dorzolamide hydrochloride was obtained with a yield of 91.2%. The purity is 99.98%, and the single impurity is less than 0.1% (HPLC see attached figure 1 ).

Example Embodiment

[0038] Example 2

[0039] This embodiment provides a method for refining dorzolamide hydrochloride, which includes:

[0040] Dissolve the crude dorzolamide hydrochloride (100 g) in water (300 g) at 85-95°C. After filtration, ethanol (300 g) was added dropwise to this aqueous solution at 40 to 45°C. The temperature was gradually cooled to 25-30°C, stirred at this temperature for 2 to 4 hours, the filter cake obtained by filtration was washed with ethanol, and dried at 50°C for 8 hours. 75.5 g of dorzolamide hydrochloride was obtained with a yield of 75.5%. The purity is 99.92%, and the single impurity is less than 0.1%.

Example Embodiment

[0041] Example 3

[0042] This embodiment provides a method for refining dorzolamide hydrochloride, which includes:

[0043] Dissolve the crude dorzolamide hydrochloride (100 g) in water (400 g) at 85-95°C. After filtration, ethanol (100 g) was added dropwise to this aqueous solution at 40 to 45°C. The temperature was gradually cooled to 25-30°C, stirred at this temperature for 2 to 4 hours, the filter cake obtained by filtration was washed with ethanol, and dried at 50°C for 8 hours. 78.2 g of dorzolamide hydrochloride was obtained with a yield of 78.2%. The purity is 99.95%, and the single impurity is less than 0.1%. (HPLC see attached figure 2 )

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Abstract

The invention relates to a refining method of dorzalamide hydrochloride, and relates to the technical field of compound purification. According to the invention, dorzalamide hydrochloride is refined by mixing water and an organic solvent; and compared with the method in the prior art, the method of the invention has advantages of high yield, high product purity, less waste treatment, simple operation, economy and environmental protection.

Description

technical field [0001] The invention relates to the technical field of compound purification, in particular to a method for refining dorzolamide hydrochloride. Background technique [0002] Dorzolamide hydrochloride, chemical name (4S-trans)-4-ethylamino-5,6-dihydro-6-methyl-4H-thieno[2,3-b]thiopyran - 2-sulfonamide-7,7-dioxide monohydrochloride, having the following formula: [0003] [0004] Dorzolamide hydrochloride, whose trade name is Trusopt, is a kind of ophthalmic solution suitable for the treatment of ocular hypertension in patients with ocular hypertension or open-angle glaucoma developed by Merck & Co., Ltd. (MSD), and has been approved by the FDA in 1994. Approved for listing. [0005] In the prior art, there is no detailed report on the refined method of dorzolamide hydrochloride, and only a little mention is made in the preparation method of dorzolamide hydrochloride. However, in the existing preparation methods, dimethyl sulfoxide or water is usually use...

Claims

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Application Information

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IPC IPC(8): C07D495/04
CPCC07D495/04
Inventor 刘传志杨波杨保姣朱毅李雷林游
Owner WUHAN WUYAO SCI & TECH
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