Cyclopropanecarboxamide derivative F crystal form and preparation method thereof

A technology of cyclopropane carboxamide and derivatives, which is applied in organic chemical methods, drug combinations, pharmaceutical formulations, etc., can solve problems such as unfavorable hygroscopicity and instability of cyclopropane carboxamide derivatives, and achieve excellent high temperature stability, good bioavailability effect

Active Publication Date: 2015-12-30
SHANGHAI SUNTRONG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The problem to be solved by the present invention is that problems such as instability, hygroscopicity and easy conversion into stable crystal forms of existing cyclopropanecarboxamide derivatives are unfavorable fo

Method used

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  • Cyclopropanecarboxamide derivative F crystal form and preparation method thereof
  • Cyclopropanecarboxamide derivative F crystal form and preparation method thereof
  • Cyclopropanecarboxamide derivative F crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0035] Example 1 Preparation of F crystal form of cyclopropanecarboxamide derivative

[0036] Weigh 500 mg of the cyclopropane carboxamide derivative raw material into a container, add 100 mL of water (analytical grade), suspend at 35°C for 48 hours, filter and vacuum dry to obtain an off-white powder. The yield was 53% by weighing.

Example Embodiment

[0037] Example 2 Preparation of F crystal form of cyclopropanecarboxamide derivative

[0038] Weigh 500mg of cyclopropanecarboxamide derivative raw material into the container, add 30mL N,N-dimethylformamide (analytical grade) to make it completely dissolved, add the resulting solution to 50mL of water (analytical grade), there is a white solid After precipitation, let it stand for 12 hours at room temperature, filter and dry in vacuum to obtain off-white powder. The yield was 56% by weighing.

Example Embodiment

[0039] Example 3. Characterization of the crystal form of cyclopropanecarboxamide derivative F by XRPD pattern

[0040] The measurement of X-ray powder diffraction (XRPD) spectrum is carried out using RigakuUltimaIV model combined multifunctional X-ray diffractometer. The specific information collected is as follows: Cu anode (40kV, 40mA), scanning speed 20° / min, scanning range (2θ range) 3~45°, scanning step length 0.02, slit width 0.01. The sample is processed by pressing the glass slide directly on the test board. The subsequent XRPD patterns adopt similar measurement methods.

[0041] The XRPD pattern of the cyclopropanecarboxamide derivative F crystal prepared according to the method described in Example 1 was determined at 2θ=7.621, 8.879, 11.061, 11.44, 14.061, 15.316, 16.08, 16.539, 17.281, 18.142, 19.859, 20.938, There are diffraction peaks at 22.299, 23.04, 23.96, 24.62, 25.121, 26.619, 28.2, 28.86, such as figure 1 Shown. The error range of 2θ value is ±0.2. After te...

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Abstract

The invention provides a cyclopropanecarboxamide derivative F crystal form (please see the specification for the formula) in the formula (I). According to the XRPD illustration of the crystal form, diffraction peaks exist when 2Q is equal to 8.717, 9.758, 10.299, 10.8, 12.879, 15.401, 16.64, 16.92, 17.859, 18.759, 19.499, 20.678, 22.841, 23.178, 23.88, 24.479, 25.958, 27.06, 28.039, 29.521 and 31.121, and the error range of the 2Q value is +/-0.2. The cyclopropanecarboxamide derivative F crystal form has good high-temperature stability, high-humidity stability and illumination stability. Moreover, low moisture absorption performance is achieved. The cyclopropanecarboxamide derivative F crystal form can be applied to drugs for treatment or prevention of JAK-participated inflammation and autoimmunity diseases, proliferative diseases, graft rejective reactions and congenital cartilage deformation or diseases caused by IL6 oversecretion, and good bioavailability is achieved. Meanwhile, qualitative and quantitative information is provided, which is of important significance to further studying the curative effect of the solid drugs.

Description

technical field [0001] The present invention relates to a polymorphic form of a cyclopropanecarboxamide derivative as a JAK inhibitor, in particular to a crystal form F of a cyclopropanecarboxamide derivative and a preparation method thereof. Background technique [0002] JAK is Janus Kinase, which is a non-receptor tyrosine protein kinase and a non-transmembrane tyrosine kinase. This is because JAK can not only phosphorylate the cytokine receptors associated with it, but also phosphorylate multiple signaling molecules containing specific SH2 domains. The JAK protein family includes 4 members: JAK1, JAK2, JAK3 and TYK2, which have 7 JAK homology domains (JAKhomology domain, JH) in their structure, of which the JH1 domain is the kinase domain and the JH2 domain is the "false" The kinase domain, JH6 and JH7 are receptor binding domains. [0003] TYK2 is a potential target for immunoinflammatory diseases, which has been confirmed by human genetics and mouse knockout studies (...

Claims

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Application Information

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IPC IPC(8): C07D471/04A61K31/541A61P37/02A61P29/00A61P35/00A61P37/06A61P19/08
CPCC07B2200/13C07D471/04
Inventor 弋东旭陈金瑶于迎渌
Owner SHANGHAI SUNTRONG BIOTECH
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