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Crystalline 4-cyanophenyl)glycine

IP.com Disclosure Number: IPCOM000234627D
Publication Date: 2014-Jan-23
Document File: 2 page(s) / 78K

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The IP.com Prior Art Database

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Crystalline 4-cyanophenyl)glycine

4-cyanophenyl)glycine of the following formula:

can be used as intermediate in the synthesis of Ethyl 3-{[(2-{[(4-{N'- [(hexyloxy)carbonyl]¬carbam¬imido¬yl}¬phenyl)amino]methyl}-1-methyl-1H-benzimidazol-5- yl)carbonyl] (2-pyridinyl)¬amino}propanoate (referred to herein as compound 1) of the following formula:

Disclosed herein is crystalline form of commercially available 4-cyanophenyl)glycine.

Crystalline form of 4-cyanophenyl)glycine

Intensity (counts)

62500

40000

22500

10000

2500

0

5

10

15

20

25

30

35

2Theta (°)

1


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Main X-Ray powder diffraction ("XRPD") peaks: 9.6, 11.7, 12.8, 15.8, 17.2, 19.3, 19.7, 21.3,


22.6, 23.1, 23.5, 25.7, 26.7, 27.9, 28.3, 28.9, 31.7, 33.0, 34.0, 34.8, 37.1, 38.3, 38.6 and 39.12- theta ± 0.2 degrees 2-theta.

XRPD method:

The X-ray diffraction was performed on X-Ray powder diffractometer:
Bruker D8 Advance; CuK_ radiation (λ = 1.5418 Å); Lynx eye detector; laboratory temperature 22-25 °C; PMMA specimen holder ring. Prior to analysis, the samples were gently ground by means of mortar and pestle in order to obtain a fine powder. The ground sample was adjusted into a cavity of the sample holder and the surface of the sample was smoothed by means of a cover glass.

Measurement parameters:

Scan range: 2 - 40 degrees 2-theta;

Scan mode: continuous;

Step size: 0.05 degrees;

Time per step: 0.5 s;

Sample spin: 30 rpm;

Sample holder: PMMA specimen holder ring. Divergence slit: V20

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