3-((L-valyl)amino)-1-propanesulfonic acid crystal form, preparation method and applications thereof

A technology of valyl and propanesulfonic acid, applied in the direction of organic chemical methods, chemical instruments and methods, preparation of organic compounds, etc.

Pending Publication Date: 2020-05-19
RISEN SUZHOU PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There is no report on the crystal form and crystal melting point of the compound 3-((L-valyl)amino)-1-propanesulfonic acid

Method used

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  • 3-((L-valyl)amino)-1-propanesulfonic acid crystal form, preparation method and applications thereof
  • 3-((L-valyl)amino)-1-propanesulfonic acid crystal form, preparation method and applications thereof
  • 3-((L-valyl)amino)-1-propanesulfonic acid crystal form, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0124] Preparation of 3-((L-valyl)amino)-1-propanesulfonic acid

[0125] 1 g of 3-((L-valyl)amino)-1-propanesulfonic acid was dissolved in 5 mL of water, and concentrated under reduced pressure to obtain 1 g of an amorphous solid compound.

[0126] The X-ray powder diffraction (XRD) pattern of this amorphous solid is shown as figure 1 shown.

Embodiment 2

[0128] Preparation of Form I of 3-((L-valyl)amino)-1-propanesulfonic acid

[0129] To 100 mg of the amorphous solid of 3-((L-valyl)amino)-1-propanesulfonic acid described in Example 1 was added a total volume of 5.0 mL of water / ethanol / acetone (1.0 ml / 2.0 ml / 2.0ml) solvent system, wherein the order of adding solvents is to add water (i.e. the first solvent) first, then add ethanol (i.e. the second solvent) and acetone (i.e. the third solvent) successively to obtain the solution, after filtration, the filtrate Placed at room temperature (crystallization temperature) to naturally evaporate to dryness to obtain 95 mg of granular crystals, which is the crystal form I. The yield is 95%, and the purity is greater than 99%.

Embodiment 3

[0131] Determination of the crystalline form I character of the 3-((L-valyl) amino)-1-propanesulfonic acid of the application embodiment 2

[0132] 1. X-ray powder diffraction of the crystal form I

[0133] Adopt the instrument, measuring method and operation condition, parameter as mentioned above to measure. The result is as figure 2 As shown, the specific data is shown in Table 1:

[0134] Table 1 figure 2 X-ray powder diffraction related data

[0135]

[0136]

[0137] 2. X-ray single crystal diffraction analysis of the crystal form I

[0138] Adopt the instrument, measuring method and operation condition, parameter as mentioned above to measure. The results are shown below and in Tables 2-3 and Figure 3-4 middle.

[0139] The molecular formula of compound 3-((L-valyl) amino)-1-propanesulfonic acid of the present invention is C 8 h 18 N 2 o 4 S, molecular weight 238.30, density 1.384Mg / m 3 , F(000)=1024. The crystal form I is a white crystal with a size...

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Abstract

The invention relates to a crystal form of a compound 3-((L-valyl)amino)-1-propanesulfonic acid, a preparation method and applications thereof.

Description

technical field [0001] The present invention relates to the crystal form of compound 3-((L-valyl)amino)-1-propanesulfonic acid, its preparation method and its use. Background technique [0002] The compound 3-((L-valyl)amino)-1-propanesulfonic acid is known to be useful in the treatment of β-amyloid-related diseases. [0003] So far, there is no report on the crystal form and crystal melting point of the compound 3-((L-valyl)amino)-1-propanesulfonic acid. [0004] Therefore, it is necessary to develop long-term storage 3-((L-valyl) amino)-1- Crystal form of propanesulfonic acid. Contents of the invention [0005] The present invention relates to a novel crystal form of compound 3-((L-valyl)amino)-1-propanesulfonic acid (hereinafter also referred to as crystal form I), which has high purity, simple preparation process, It has good thermodynamic stability, low hygroscopicity, good flow properties, good reproducibility in manufacturing, meets the quality requirements of ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/44C07C309/15A61K31/198A61P25/28A61P9/10
CPCC07C303/44C07C309/15A61P25/28A61P9/10C07B2200/13A61P25/00C07B2200/07
Inventor 吕佳声顾家敏吉祥吕新勇彭娟孔宪起
Owner RISEN SUZHOU PHARMA TECH CO LTD
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