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Amorphous crystal form of acetylcholine chloride and preparation method thereof

An amorphous technology of methacholine chloride, which is applied in the field of pharmaceutical crystal forms, can solve the problems of easy deliquescence of methacholine chloride and excessive water content, and achieve convenient production and quality control, strong wet stability, The effect of high yield

Pending Publication Date: 2020-09-08
北京磐谷英汇科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The first object of the present invention is to provide an amorphous form of methacholine chloride and a preparation method thereof, so as to solve the problem that methacholine chloride is easy to deliquesce and the moisture is easy to exceed the standard in the prior art

Method used

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  • Amorphous crystal form of acetylcholine chloride and preparation method thereof
  • Amorphous crystal form of acetylcholine chloride and preparation method thereof
  • Amorphous crystal form of acetylcholine chloride and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The preparation method of the methacholine chloride amorphous crystal form described in the present embodiment, the steps are as follows:

[0034] First group:

[0035] (a) Weigh 100g of the crude methacholine chloride, put it in a container, add 100mL of acetonitrile to stir, slowly raise the temperature to 45-55°C, the crude methacholine chloride is not completely dissolved, take the acetonitrile and slowly add it dropwise to the system During the process, the dropwise addition of acetonitrile was stopped when the system just became clear, and the recorded dropwise amount of acetonitrile was 96 mL.

[0036] (b) Keep the solution system in (a) at 45-55°C, slowly add ethyl acetate dropwise to the system, stop adding ethyl acetate dropwise when the system starts to become cloudy, and record the amount of ethyl acetate dropwise as 352mL , stop heating.

[0037] (c) Continue to stir the cloudy solution in (b) to room temperature, then lower the temperature to 0-5°C and s...

Embodiment 2

[0050] The preparation method of the methacholine chloride amorphous crystal form described in the present embodiment, the steps are as follows:

[0051] First group:

[0052] (a) Weigh 100g of the crude methacholine chloride, place it in a container, add 200mL of n-butanol to stir, slowly raise the temperature to 45-55°C, the crude methacholine chloride is not completely dissolved, take n-butanol and slowly Add it dropwise to the system, stop adding n-butanol when the system just becomes clear, record the amount of n-butanol added dropwise as 88mL.

[0053] (b) Keep the solution system in (a) at 45-55°C, slowly add ethyl acetate dropwise to the system, stop adding ethyl acetate dropwise when the system starts to become cloudy, and record the amount of ethyl acetate dropwise as 278mL , stop heating.

[0054] (c) Continue to stir the cloudy solution in (b) to room temperature, then lower the temperature to 0-5°C and stir for 3 hours to precipitate crystals. The suspension wa...

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PUM

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Abstract

The invention relates to the technical field of medicine crystal forms, in particular to an amorphous crystal form of methylcholine chloride and a preparation method of the amorphous crystal form. Inan X-ray powder diffraction pattern of the amorphous acetylcholine chloride crystal form, an amorphous characteristic steamed bun peak exists when 2 theta is equal to 20-35 when the X-ray powder diffraction pattern is expressed by 2 theta + / -0.2 degrees. The preparation method comprises the following steps: dissolving a crude product of acetylcholine chloride in acetonitrile or n-butyl alcohol, and dropwise adding ethyl acetate, acetone or tetrahydrofuran to obtain the amorphous crystal form of acetylcholine chloride. The amorphous crystal form has better wet stability, thereby being beneficial to production and quality control of bulk drugs.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical crystal forms, in particular to an amorphous crystal form of methacholine chloride and a preparation method thereof. Background technique [0002] Methacholine chloride, also known as methacholine, is a white highly hygroscopic crystal with a light smell of dead fish. Its molecular formula is C 8 h 18 ClNO 2 . It can excite M choline receptors, has a strong selectivity to the cardiovascular system, and has a weak effect on the smooth muscle of the gastrointestinal tract and bladder. It can also contract bronchial smooth muscle and increase bronchial secretion. [0003] Methacholine chloride is very sensitive to moisture, it is easy to absorb moisture and agglomerate or deliquescence into liquid, which is not conducive to storage. Due to this characteristic in the production of raw materials, it brings great inconvenience to the production, especially in the refining process. At the sam...

Claims

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Application Information

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IPC IPC(8): C07C219/06C07C213/10
CPCC07C219/06C07B2200/13
Inventor 李晓曦唐金龙
Owner 北京磐谷英汇科技有限公司
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