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Cyclopropanecarboxamide derivative E crystal form and preparation method thereof

A cyclopropanecarboxamide and derivative technology, applied in organic chemical methods, drug combinations, pharmaceutical formulations, etc., can solve problems such as unfavorable hygroscopicity and instability of cyclopropanecarboxamide derivatives, and achieve excellent high temperature stability, The effect of good solubility and low hygroscopicity

Active Publication Date: 2015-12-02
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 for pharmaceutical processing and use in pharmaceutical compositions. Cyclopropanecarboxamide derivatives The problem of providing more qualitative and quantitative information for the curative effect research of solid drugs

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Embodiment 1 Preparation of cyclopropanecarboxamide derivative E crystal form

[0039] Weigh 500 mg of cyclopropanecarboxamide derivative raw material into a container, add 15 mL of N,N-dimethylformamide (analytical grade), sonicate at room temperature for 30 min, filter, and vacuum-dry to obtain off-white powder. Its yield of weighing calculation is 71%.

Embodiment 2

[0040] Embodiment 2 Preparation of cyclopropanecarboxamide derivative E crystal form

[0041] Weigh 500 mg of cyclopropanecarboxamide derivative raw material in a container, add 10 mL of dimethyl sulfoxide (analytical grade) to dissolve it completely, add the resulting solution to 50 mL of 2-butanone (analytical grade), a white solid precipitates out , standing at room temperature for 12 hours, filtered, and vacuum-dried to obtain off-white powder. Its yield of weighing calculation is 66%.

Embodiment 3

[0042] Embodiment 3. Characterize cyclopropanecarboxamide derivative E crystal form by XRPD pattern

[0043] The measurement of the X-ray powder diffraction (XRPD) pattern is carried out using the RigakuUltimaIV model combined multifunctional X-ray diffractometer, and the specific collection information is as follows: Cu anode (40kV, 40mA), scanning speed 20° / min, scanning range (2θ range) 3~45°, scan step size 0.02, slit width 0.01. Samples were processed using glass slides pressed directly onto the test plate. Subsequent XRPD patterns all adopt similar measurement methods.

[0044] Determination of the XRPD spectrum of the cyclopropanecarboxamide derivative E crystal form prepared according to the method described in Example 1, at 2θ=8.717, 9.758, 10.299, 10.8, 12.879, 15.401, 16.64, 16.92, 17.859, 18.759, 19.499, 20.678, There are diffraction peaks at 22.841, 23.178, 23.88, 24.479, 25.958, 27.06, 28.039, 29.521, and 31.121, such as figure 1 shown. The error range of 2θ va...

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Abstract

The invention provides a cyclopropanecarboxamide derivative E crystal form (please see the formula in the specification). According to the XRPD map of the cyclopropanecarboxamide derivative E crystal form, diffraction peaks exist at the positions of 2theta=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, wherein the error range of the 2theta values is + / -0.2. The cyclopropanecarboxamide derivative E crystal form has good high-temperature stability and illumination stability and also has low moisture absorption performance and good solubility, can be applied to drugs for treating or preventing inflammations where JAK takes part in, autoimmune diseases, proliferative diseases, transplant rejection reaction, congenital cartilage deformity or diseases caused by IL6 hypersecretion, and has good bioavailability, and meanwhile the provided qualitative and quantitative information has great significance for further study of the curative effect of the kind of solid drugs.

Description

technical field [0001] The invention relates to a polymorphic form of a cyclopropanecarboxamide derivative as a JAK inhibitor, in particular to a cyclopropanecarboxamide derivative E crystal form 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 (Levy D. and L...

Claims

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Application Information

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IPC IPC(8): C07D471/04A61K31/541A61P35/00A61P29/00A61P37/02A61P37/06A61P3/02A61P19/08
CPCC07B2200/13C07D471/04
Inventor 弋东旭陈金瑶于迎渌
Owner SHANGHAI SUNTRONG BIOTECH