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Crystalline forms of Sodium salt of N-propylsulfamide

IP.com Disclosure Number: IPCOM000241076D
Publication Date: 2015-Mar-25
Document File: 6 page(s) / 494K

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Page 01 of 6

Crystalline forms of Sodium salt of N-propylsulfamide

Sodium salt of N-propylsulfamideis an intermediate in Macitentan synthesis

Figure 1. Molecular structure of Sodium salt of N-propylsulfamide


Page 02 of 6

Sodium salt of N-propylsulfamide crystalline form II.

List of XRD peaks: 5.7, 6.3, 7.5, 11.4, 17.1, 17.8, 19.0, 25.0, 25.4 and 28.8° ±0.2° 2θ.

Intensity (counts)

90000

40000

10000

0

5 10 15 20 25 30 35 2Theta (°)

Figure 2. PXRD pattern of Sodium salt of N-propylsulfamide crystalline form II.


Page 03 of 6

Sodium salt of N-propylsulfamidecrystalline form III.

List of XRD peaks: 5.1, 5.5, 6.3, 12.6, 16.2, 18.6, 19.6, 20.1, 20.7, 21.2, 22.1, 23.6, 24.7,
25.4, 27.8, 28.1, 29.4, 31.0, 33.4 and 34.3° ±0.2° 2θ.

Intensity (counts)

250000

160000

90000

40000

10000

0

5 10 15 20 25 30 35 2Theta (°)

Figure 3. PXRD pattern of Sodium salt of N-propylsulfamide crystalline form III.

Figure 4. FTIR spectrum of Sodium salt of N-propylsulfamide crystalline form III.


Page 04 of 6

Sodium salt of N-propylsulfamide crystalline form IV.

List of XRD peaks: 5.2, 5.7, 6.3, 8.9, 12.6, 16.2, 19.0, 19.6, 24.7, 25.4, 28.1, 29.4, 31.9, 33.4 and 38.5° ±0.2° 2θ.

1440000

Intensity (counts)

1000000

640000

360000

160000

40000

0

5 10 15 20 25 30 35 2Theta (°)

Figure 5. PXRD pattern of Sodium salt of N-propylsulfamide crystalline form IV.

Figure 6. FTIR spectrum of Sodium salt of N-propylsulfamide crystalline form IV.


Page 05 of 6

Experimental:

PXRD method:

After being powdered using mortar and pestle, samples were applied directly on a silicon plate holder. The X-ray powder diffraction pattern was measured with a Philips X'Pert PRO X-ray powder diffractometer, equipped with a Cu irradiation source = 1.54184 Ǻ (Ǻngström), X'Celerator (2.022º 2θ) detector. Scanning parameters: angle range: 3-40 deg., step size
0.0167, time per step 37 s, continuous scan. The accuracy of peak positions was defined as +/-
0.2 degrees due to experimental differences like instrumentations and sample preparations.

FTIR me...