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A crystalline form of (S)-1-(3-hydroxypiperidin-1-yl)prop-2-en-1-one

IP.com Disclosure Number: IPCOM000237037D
Publication Date: 2014-May-28
Document File: 2 page(s) / 18K

Publishing Venue

The IP.com Prior Art Database

This text was extracted from a PDF file.
This is the abbreviated version, containing approximately 57% of the total text.

Page 01 of 2

A crystalline form of (S)-1-(3-hydroxypiperidin-1-yl)prop-2-en-1-one

     Provided herein is a process for preparing a crystalline form of (S)-1-(3- hydroxypiperidin-1-yl)prop-2-en-1-one, referred herein as Compound I. The process is described in Example 1. The isolated samples were analyzed by X-ray powder diffraction ("XRPD"), which indicated a formation of a crystalline form of Compound
I. Figure 1 depicts the XRPD of the obtained crystalline form.

    Compound I may be used for preparing (S)-1-(3-(4-amino-3-(4- phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl)piperidin-1-yl)prop-2-en-1-one.

Figure 1: XRPD of a crystalline form of Compound I CPS

°2 theta

    
According to Figure 1, the crystalline form of Compound I is characterized by XRPD peaks at: 7.3, 13.3, 14.6, 16.8, 18.5, 19.5, 21.2, 22.2, 22.5, 23.4, 24.8, 25.7,
25.9, 26.7, 28.9, 29.6, 32.3, 33.5, 35.0, 35.8, 37.2, 38.2 and 39.7 degrees 2-theta ± 0.2 degrees 2-theta.

XRPD method:

    The analysis was performed on ARL (SCINTAG) powder X-Ray diffractometer model X'TRA equipped with a solid state detector. Copper radiation of
1.5418 Å was used. Scanning parameters: range: 2-40 degrees two-theta; scan mode: continuous scan; step size: 0.05°, and a rate of 3 deg/min.

10000

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2.0


6.0


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14.0


18.0


22.0


26.0


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34.0


38.0


Page 02 of 2

Example 1: A process for preparing a crystalline form of (S)-1-(3- hydroxypiperidin-1-yl)prop-2-en-1-one

    Flask (4 L) equipped with overhead stirrer, thermometer and droppin...