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N-(2-(6-fluoro-1H-indol-3-yl)ethyl-3-(2,2,3,3-tetrafluoropropoxy) benzylamine acetate salt

IP.com Disclosure Number: IPCOM000247733D
Publication Date: 2016-Oct-02
Document File: 2 page(s) / 250K

Publishing Venue

The IP.com Prior Art Database

This text was extracted from a PDF file.
This is the abbreviated version, containing approximately 62% of the total text.

Page 01 of 2

-

N

-

(2

-

(6

-

fluoro

indol

-

1H

-

-

3

yl)ethyl

-

-

3

(2,2,3,3

-

tetrafluoropropoxy)

benzylamine

acetate

salt

Provided herein is a process for preparing crystalline form 2 of N-(2-(6-fluoro-1H-indol-3- yl)ethyl-3-(2,2,3,3-tetrafluoropropoxy)benzylamine acetate salt. Crystalline form 2 of N-(2- (6-fluoro-1H-indol-3-yl)ethyl-3-(2,2,3,3-tetrafluoropropoxy)benzylamine acetate salt can be prepared according to example 1 or 2.

EXAMPLE-1

N-(2-(6-fluoro-1H-indol-3-yl)ethyl-3-(2,2,3,3-tetrafluoropropoxy)benzylamine HCl Form-I
0.5 gm was added to 50ml of 0.02 molar sodium acetate solution in water which was adjusted to pH 4.5 with 2 normal acetic acid at 20-25ºC and the obtained slurry was stirred for 18 hours. The obtained solid was filtered under vacuum and kept under suction for about 20 minutes to obtain solid was about 0.56 gm.

EXAMPLE-2

N-(2-(6-fluoro-1H-indol-3-yl)ethyl-3-(2,2,3,3-tetrafluoropropoxy)benzylamine HCl Form-I
0.5 gm was added to 50ml of 0.02 molar sodium acetate solution in water which was adjusted to pH 4.5 with 2 normal acetic acid at 20-25ºC and the obtained slurry was stirred for 56 hours. The obtained solid was filtered under vacuum and kept under suction for about 20 minutes to obtain solid was about 0.45 gm.

Figure 1 shows a powder X-ray diffraction pattern ("powder XRD" or "PXRD") of Form-2 of N-(2-(6-fluoro-1H-indol-3-yl)ethyl-3-(2,2,3,3-tetrafluoropropoxy)benzylamine acetate salt. Characteristic peaks are at 8.3; 9.5; 11.8; 14.4; 16.7 21.0;...