Dismiss
InnovationQ will be updated on Sunday, Oct. 22, from 10am ET - noon. You may experience brief service interruptions during that time.
Browse Prior Art Database

Crystalline (3R,11bR) – 3 – isobutyl - 9,10 – dimethoxy - 1,3,4,6,7,11b - hexahydro-2H-pyrido[2,1-a]isoquinolin-2-one

IP.com Disclosure Number: IPCOM000247034D
Publication Date: 2016-Jul-28
Document File: 1 page(s) / 174K

Publishing Venue

The IP.com Prior Art Database

This text was extracted from a PDF file.
This is the abbreviated version, containing approximately 100% of the total text.

Page 01 of 1

Crystalline (3R,11bR) - 3 - isobutyl - 9,10 - dimethoxy - 1,3,4,6,7,11b - hexahydro-2H-pyrido[2,1-a]isoquinolin-2-one

Disclosed herein is a crystalline form of (3R,11bR)-3-isobutyl-9,10-dimethoxy- 1,3,4,6,7,11b-hexahydro-2H-pyrido[2,1-a]isoquinolin-2-one ("compound I"). Preparation of crystalline form of Compound I was conducted as described in European Journal of Medicinal Chemistry, 2011, 46, 1841-1848. (Based on Exp# TN-7308).

The obtained crystalline product was characterized by XRPD. The XRPD pattern is presented in the following representative X-ray diffractogram):

Sample ID: Analyst: Firas, Sample name: VLB TN-7308+SI, Temp: 25.0°C
Date: 07/19/16 18:22 Step : 0.050° Integration Time: 1.000 sec
Range: 2.000 - 40.000° Cont. Scan Rate: 3.000 [°/min]

Vert. Scale Unit: [CPS]

Horz. Scale Unit: [deg]

60000

50000

40000

30000

20000

10000

Si

0


2.0


6.0


10.0


14.0


18.0


22.0


26.0


30.0


34.0


38.0

XRPD peaks: 6.4, 8.6, 10.0, 12.0, 12.2, 14.0, 14.9, 16.4, 17.3, 17.8, 18.5,
19.9, 20.6, 22.5, 23.1, 23.4, 24.0, 24.4, 25.2, 26.2 and 28.8 ± 0.2 degrees 2- theta.

XRPD 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. The peak at about 28.5° is attributed to silicon powder added as an internal standard for peak position.