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

IP.com Disclosure Number: IPCOM000247033D
Publication Date: 2016-Jul-28
Document File: 1 page(s) / 212K

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

Disclosed herein is a crystalline form of (2R,3R,11bR)-3-isobutyl-9,10- dimethoxy-1,3,4,6,7,11b-hexahydro-2H-pyrido[2,1-a]isoquinolin-2-ol ("compound I").

Preparation of crystalline form of Compound I was conducted as described in Synthetic Communications, 2009, 39, 3574-3585. (Based on Exp# TN-7409). 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-1 TN-7409, Temp: 25.0°C

Date: 07/17/16 11:42 Step : 0.050° Integration Time: 1.000 sec

Vert. Scale Unit: [CPS]

Range: 2.000 - 40.000° Cont. Scan Rate: 3.000 [°/min]

Horz. Scale Unit: [deg]

5000

4000

3000

2000

1000

0


2.0


6.0


10.0


14.0


18.0


22.0


26.0


30.0


34.0


38.0

XRPD peaks: 6.0, 6.8, 8.9, 11.3, 12.5, 12.9, 13.5, 14.2, 15.8, 17.0, 18.0, 18.7,
19.8, 20.2, 20.8, 21.3, 22.0, 22.6, 23.1, 23.5, 24.0, 24.8, 25.2, 26.7, 26.9,
27.3, 27.6, 28.0, 28.6, 28.9 and 29.7 ± 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.