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A kind of cyclopropanecarboxamide derivative H crystal form and preparation method thereof

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

Active Publication Date: 2017-09-29
SHANGHAI SUNTRONG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of cyclopropanecarboxamide derivative H crystal form and preparation method thereof
  • A kind of cyclopropanecarboxamide derivative H crystal form and preparation method thereof
  • A kind of cyclopropanecarboxamide derivative H crystal form and preparation method thereof

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Effect test

Embodiment 1

[0033] Embodiment 1 Preparation of cyclopropanecarboxamide derivative H crystal form

[0034] Weigh 500 mg of cyclopropanecarboxamide derivative raw material into a container, add 100 mL of ethanol (analytical grade) and N,N-dimethylformamide (analytical grade) 1:2 mixed solvent, suspend at 35°C for 48 hours, filter , Vacuum drying to obtain off-white powder. Its yield of weighing calculation is 56%.

Embodiment 2

[0035] Embodiment 2. Characterize cyclopropanecarboxamide derivative H crystal form by XRPD pattern

[0036] The measurement of the X-ray powder diffraction (XRPD) pattern is carried out using the Rigaku UltimaIV 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.

[0037] Determination of the XRPD spectrum of the cyclopropanecarboxamide derivative H crystal form prepared according to the method described in Example 1, at 2θ=9.341, 13.019, 14.2, 16.66, 17.201, 18.37, 18.901, 20.522, 20.82, 21.141, 21.759, 23.001, There are diffraction peaks at 23.441, 24.461, 25.059, 26, 26.539, 28.8, 29.661, and 33.657, such as figure 1 shown. The error range of 2θ value is ±0...

Embodiment 3

[0039] Example 3. Investigation of High Temperature Stability of Cyclopropanecarboxamide Derivative H Crystal Form

[0040] The cyclopropanecarboxamide derivative H crystal sample was placed in a 60°C oven, and after 5 days and 10 days, the samples were taken out for XRPD testing (such as figure 2 and Figure 5 Shown), in order to investigate the stability of the crystal form of the sample to temperature. The results show that the crystal form H sample is stable under high temperature conditions.

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Abstract

The invention provides a cyclopropanecarboxamide derivative H 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 9.341, 13.019, 14.2, 16.66, 17.201, 18.37, 18.901, 20.522, 20.82, 21.141, 21.759, 23.001, 23.441, 24.461, 25.059, 26, 26.539, 28.8, 29.661 and 33.657, and the error range of the 2Q value is + / -0.2. The cyclopropanecarboxamide derivative H crystal form has good high-temperature stability, high-humidity stability and illumination stability. Moreover, low moisture absorption performance is achieved. The cyclopropanecarboxamide derivative H 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 further 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 invention relates to a polymorphic form of a cyclopropanecarboxamide derivative as a JAK inhibitor, in particular to a cyclopropanecarboxamide derivative H crystal form and a preparation method thereof. Background technique [0002] JAK, Janus Kinase, 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 consists of four members: JAK1, JAK2, JAK3 and TYK2, which have seven JAK homology domains (JAK homology domain, JH) in structure, of which the JH1 domain is the kinase domain and the JH2 domain is the " The "pseudo" kinase domain, JH6 and JH7, are receptor binding regions. [0003] TYK2 is a potential target for immunoinflammatory diseases, which has been confirmed by human genetics and mouse knockout studies (Levy D. and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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