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A CRYSTALLINE FORM OF (R)-6-HYDROXY-8-{1-HYDROXY-2-[2-(4-METHOXYPHENYL)-1,1-DIMETHYLETHYLAMINO]ETHYL}-4H-BENZO[1,4]OXAZIN-3-ONE HYDROCHLORIDE

IP.com Disclosure Number: IPCOM000247884D
Publication Date: 2016-Oct-10
Document File: 4 page(s) / 497K

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A CRYSTALLINE FORM OF (R)-6-HYDROXY-8-{1-HYDROXY-2-[2-(4- METHOXYPHENYL)-1,1-DIMETHYLETHYLAMINO]ETHYL}-4H-

BENZO[1,4]OXAZIN-3-ONE HYDROCHLORIDE

    Described herein is a crystalline form of (R)‐6‐hydroxy‐8‐{1‐hydroxy‐2‐[2‐(4‐ methoxyphenyl)‐1,1‐dimethylethylamino]ethyl}‐4H‐benzo[1,4]oxazin‐3‐one hydrochloride, referred herein as compound A. The crystalline form of Compound A is an anhydrous.

Samples of Compound A were prepared according to the process described in example 1

below, and were analyzed by X-ray powder diffraction ("XRPD"), Thermogravimetric

analysis ("TGA"), Differential scanning calorimetry ("DSC"). Figures 1-3 present the XRPD,

TGA and DSC of the obtained form.

Figure 1: XRPD pattern of the crystalline form of Compound A:

The crystalline form of Compound A is characterized by XRPD peaks as provided in the table below ( ± 0.2 deg. 2θ):

Pos. [°2θ]

Intensity (cps)

500

400

300

200

100

0

5 10 15 20 25 30 35 40 2Theta (°)

d-spacing


[Å]

Rel. Int. [%]


9.3 9.53 10.3
10.6 8.35 9.1
12.5 7.10 12.5
13.4 6.60 12.5
14.9 5.94 79.8
15.2 5.83 100.0
16.0 5.53 24.4
16.9 5.25 24.1
17.4 5.11 29.3
17.8 4.97 20.5
18.6 4.78 15.6

19.1 4.66 22.1
19.7 4.50 28.5
21.0 4.23 13.1
21.4 4.16 97.5
21.6 4.12 33.8
22.2 4.01 70.9
22.6 3.94 1.6
23.0 3.87 10.4
23.2 3.83 21.1
23.7 3.75 3.0
24.4 3.65 14.4
24.4 3.65 11.3


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24.9 3.57 5.3
25.0 3.55 11.3
25.3 3.51 2.2
25.8 3.45 13.0
26.0 3.42 4.5
26.7 3.34 15.8
27.3 3.26 5.1
27.9 3.20 5.4
28.1 3.17 5.4
28.4 3.14 13.3
29.2 3.06 19.6
29.4 3.03 6.4
29.8 3.00 25.9
30.1 2.97 12.2
30.1 2.97 8.3
30.5 2.93 30.7
30.6 2.92 27.7
30.7 2.91 17.7
31.4 2.85 16.6
31.6 2.83 14.6

32.0 2.79 7.1
32.2 2.78 4.7
32.8 2.72 3.8
33.3 2.69 3.8
33.4 2.68 6.8
33.6 2.66 5.6
34.5 2.60 4.4
34.8 2.58 0.9
35.0 2.56 3.8
35.8 2.51 4.0
36.1 2.49 8.2
36.2 2.48 9.0
36.7 2.45 19.2
37.4 2.40 7.9
37.7 2.38 6.3
38.0 2.37 6.5
38.2 2.36 4.1
38.7 2.32 7.2
39.0 2.31 4.8

Figure 2: TGA graph of the crystalline form of Compound A:


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