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Preparation method of L-lysine hydrochloride beta crystal form

A technology of lysine hydrochloride and β crystal form, which is applied in the field of preparation of L-lysine hydrochloride β crystal form, can solve the problems of cumbersome operation and unfavorable industrial production, and achieve the effect of avoiding mixed crystals

Active Publication Date: 2021-04-20
北京民康百草医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both of these two methods need to go through three drying stages, and both need to be fed with saturated steam. The operation is relatively cumbersome, which is not conducive to industrial production.

Method used

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  • Preparation method of L-lysine hydrochloride beta crystal form
  • Preparation method of L-lysine hydrochloride beta crystal form
  • Preparation method of L-lysine hydrochloride beta crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1: preparation embodiment

[0039] Take 200g of L-lysine hydrochloride, add 400ml of purified water to dissolve, add 10g of activated carbon, heat to 80-90°C, decolorize for 30min, filter and decarburize, concentrate at 60-70°C for 3h to 20°Bé, cool to 5-15°C ℃, crystallized for 3 hours, and filtered to obtain 150 g of L-lysine hydrochloride dihydrate. Get sample (1) to detect XRD and DSC, the results are as follows figure 1 , figure 2 shown.

Embodiment 2

[0040] Embodiment 2: comparison preparation embodiment

[0041] Put 150 g of L-lysine hydrochloride dihydrate prepared according to Example 1 into a forced air drying oven at 105° C. for 2 hours to obtain L-lysine hydrochloride anhydrate. Get sample (2) to detect XRD and DSC, the results are as follows image 3 (shown as α crystal form, XRD pattern has a diffraction angle at 4.5°), Figure 4 shown.

Embodiment 3

[0042] Embodiment 3: preparation embodiment

[0043] Put 148 g of L-lysine hydrochloride dihydrate prepared according to Example 1 into a three-neck flask, and heat at 80°C for 2 hours to obtain the intermediate transition state crystal form of L-lysine hydrochloride. XRD and DSC were detected, and the result Respectively as Figure 5 , Figure 6 shown. The intermediate transition state crystal form was transferred to a forced air drying oven at 105° C. for 2 hours to obtain L-lysine hydrochloride. Get sample (3) to detect XRD and DSC, the results are as follows Figure 7 (shown as β crystal form, XRD pattern has no diffraction angle at 4.5°), Figure 8 shown.

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Abstract

The invention belongs to the technical field of crystal form medicines, and relates to a preparation method of an L-hydrochloric acid lysine beta-crystal form. The preparation method comprises the following steps: (1) heating and concentrating a solution obtained by dissolving L-lysine hydrochloride in water, cooling, crystallizing and filtering to obtain L-lysine hydrochloride dihydrate; (2) heating the L-lysine hydrochloride dihydrate in a closed system or a semi-closed system to obtain an intermediate transition state crystal form of L-lysine hydrochloride; and (3) drying the intermediate transition state crystal form to obtain the medicinal L-lysine beta hydrochloride crystal form. By utilizing the preparation method of the L-lysine hydrochloride beta crystal form, common equipment in a laboratory or a bulk drug workshop can be used for stably producing the L-lysine hydrochloride beta crystal form, and the generation of mixed crystals is avoided.

Description

technical field [0001] The invention belongs to the technical field of crystal form drugs, and relates to a preparation method of L-lysine hydrochloride β crystal form. Background technique [0002] L-Lysine hydrochloride, whose structure is shown below, is widely used in the pharmaceutical, food and feed industries to supplement the body with lysine or improve the performance of certain drugs. [0003] [0004] A variety of hydrates, crystal forms and preparation methods of L-lysine hydrochloride have been reported in the literature, including lysine hydrochloride trihydrate, dihydrate, monohydrate; α crystal form, β crystal form, of which the medicinal L - Lysine hydrochloride in the beta crystal form of anhydrous. [0005] U.S. Patent US4256917 reported that L-lysine hydrochloride dihydrate was prepared by heating to obtain a new crystal form, which is anhydrous α crystal form, and its preparation is related to the content of sodium ions or the temperature of dehydrat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/40C07C227/42C07C229/26
Inventor 刘云涛严智王军刘磊陈伟王晓波
Owner 北京民康百草医药科技有限公司