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One-pot method for preparing sarpogrelate hydrochloride photodegradation impurities I, II, III and IV

A technology of sarcogrelate hydrochloride and photodegradation, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., can solve the problems of low efficiency and achieve high efficiency, few steps, and high utilization of raw materials Effect

Active Publication Date: 2017-11-10
绍兴市逸晨医疗科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, the above-mentioned four kinds of impurities are prepared by four different synthesis processes, and each has multi-step reactions, and the efficiency is low

Method used

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  • One-pot method for preparing sarpogrelate hydrochloride photodegradation impurities I, II, III and IV
  • One-pot method for preparing sarpogrelate hydrochloride photodegradation impurities I, II, III and IV

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 Preparation and Separation of Photodegradation Impurities I, II, III, and IV

[0026] Preparation method of degradation mixture:

[0027] Dissolve 60mg of sargrelate hydrochloride in water to prepare a 3mg / mL solution, heat it at 85°C for 1.5 hours, and then irradiate it with 1,200,000 lux cool white fluorescent lamps for 5 hours and 200 Wh / m2 ultraviolet fluorescent lamps After irradiating for 4 hours, the degraded solution was concentrated and frozen until dry to obtain a degraded mixture.

[0028] High-speed countercurrent separation of degradation mixtures:

[0029] Prepare the ethyl acetate-ethanol-water-formic acid (4:1:5:0.025, v / v / v / v) solvent system 12 hours before the separation. The specific preparation method is: mix the four solvents in proportion, and shake vigorously , let it stand for 12 hours to completely separate the upper and lower phases in the funnel, the upper phase is used as a stationary phase, and the lower phase is used as a mobile...

Embodiment 2

[0033] Example 2 Preparation and separation of photodegradation impurities Ⅰ, Ⅱ, Ⅲ, Ⅳ

[0034] Preparation method of degradation mixture:

[0035] Dissolve 60mg of sargrelate hydrochloride in water to prepare a 2mg / mL solution, heat it at 80°C for 2 hours, and then irradiate it with 1,200,000 lux cool white fluorescent lamps for 4 hours, 200 Wh / m2 ultraviolet fluorescent lamps After irradiating for 5 hours, the degraded solution was concentrated and frozen until dry to obtain a degraded mixture.

[0036] High-speed countercurrent separation of degradation mixtures:

[0037] Prepare the ethyl acetate-ethanol-water-formic acid (4:1:5:0.025, v / v / v / v) solvent system 12 hours before the separation. The specific preparation method is: mix the four solvents in proportion, and shake vigorously , let it stand for 12 hours to completely separate the upper and lower phases in the funnel, the upper phase is used as a stationary phase, and the lower phase is used as a mobile phase, and u...

Embodiment 3

[0041] Example 3 Preparation and Separation of Photodegradation Impurities I, II, III, and IV

[0042] Preparation method of degradation mixture:

[0043] Take 60mg of sargrelate hydrochloride and dissolve it in water to prepare a 4mg / mL solution, heat it at 90°C for 1 hour, and then irradiate it with 1,200,000 lux cool white fluorescent lamp for 6 hours, 200 Wh / m2 ultraviolet fluorescent lamp After irradiating for 3 hours, the degraded solution was concentrated and frozen until dry to obtain a degraded mixture.

[0044] High-speed countercurrent separation of degradation mixtures:

[0045] Prepare the ethyl acetate-ethanol-water-formic acid (4:1:5:0.025, v / v / v / v) solvent system 12 hours before the separation. The specific preparation method is: mix the four solvents in proportion, and shake vigorously , let it stand for 12 hours to completely separate the upper and lower phases in the funnel, the upper phase is used as a stationary phase, and the lower phase is used as a mo...

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Abstract

The invention discloses a one-pot method for preparing sarpogrelate hydrochloride photodegradation impurities I, II, III and IV. The method comprises the steps as follows: S1, photodegradation: 2-4 mg / mL of a solution is prepared by dissolving sarpogrelate hydrochloride in water, is treated at the high temperature of 80-90 DEG C for 1-2 h and then sequentially irradiated by a 1200,000-lux cold white fluorescent lamp for 4-6 h and a 200 Wh / m<2> ultraviolet fluorescent lamp for 3-5 h, finally, the degraded solution is concentrated and frozen to dryness, and a degraded mixture is obtained; S2, high-speed countercurrent chromatography: the degraded mixture is dissolved with a fixed phase and a mobile phase with the same volume to serve as a sample solution, ethyl acetate-ethanol-water-formic acid (4:1:5:0.025, v / v / v / v) serves as a two-phase solvent system, the upper phase is the fixed phase, the lower phase is the mobile phase, and the impurities I, II, III and IV are prepared through one-time separation under the conditions that the main engine rotational speed is 800 r / min, the flow velocity is 2.0 mL / min and the detection wavelength is 272 nm. The method adopts few steps and has high efficiency.

Description

technical field [0001] The invention belongs to the field of medicines and relates to a method for preparing sargrelate hydrochloride by photodegrading impurities I, II, III and IV in one pot. Background technique [0002] Sagrelate Hydrochloride Tablets was first launched in Japan in 1993 under the trade name of Anplag. It is a 5-HT2 receptor blocker that can inhibit platelet aggregation and vasoconstriction, has antithrombotic effect and improves microcirculation. Its indications are to improve ischemic symptoms such as ulcers, pain and cold sensation caused by chronic arterial occlusive disease. [0003] The quality research of sarcogrelate hydrochloride bulk drug involves the following four kinds of photodegradation impurities: [0004] [0005] In the prior art, the above-mentioned four kinds of impurities are prepared through four different synthesis processes, and each has multi-step reactions, so the efficiency is low. Contents of the invention [0006] The pu...

Claims

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Application Information

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IPC IPC(8): C07C213/00C07C213/08C07C213/10C07C217/32C07C219/06
CPCC07C213/00C07C213/08C07C213/10C07C217/32C07C219/06
Inventor 陈云薛鹏宇王斌
Owner 绍兴市逸晨医疗科技有限公司
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