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A crystalline form of L-valine (2R,3R,11bR)-1,3,4,6,7,11b-hexahydro-9,10-dimethoxy-3-(2-methylpropyl)-2H-benzo[a]quinolizin-2-yl ester

IP.com Disclosure Number: IPCOM000247708D
Publication Date: 2016-Sep-28
Document File: 2 page(s) / 275K

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A crystalline form of L-valine (2R,3R,11bR)-1,3,4,6,7,11b-hexahydro-9,10- dimethoxy-3-(2-methylpropyl)-2H-benzo[a]quinolizin-2-yl ester

     Provided herein is a process for preparing crystalline form of L-valine (2R,3R,11bR)-1,3,4,6,7,11b-hexahydro-9,10-dimethoxy-3-(2-methylpropyl)-2H- benzo[a]quinolizin-2-yl ester, referred herein as Compound I. The process is described in Example 1.

Example 1: A process for preparing a crystalline form of L-valine (2R,3R,11bR)- 1,3,4,6,7,11b-hexahydro-9,10-dimethoxy-3-(2-methylpropyl)-2H- benzo[a]quinolizin-2-yl ester (Compound I)

    Compound I was charged in glass vial with magnetic stir (36mg) and dimethylacetamide (20µL) .The obtained slurry was heated to 70°C and clear solution was obtained. Water (215 µL) was added and precipitation was observed. The obtained slurry was stirred for 2 hours and then filtrated. The obtained solid was analyzed by X- ray powder diffraction ("XRPD") to provide a crystalline form as depicted in figure 1.

XRPD

The 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 main XRPD peaks are: 6.0, 6.8,
8.4, 9.9, 11.3, 12.0, 13.5, 14.3, 15.3, 16.4, 16.8, 17.2, 17.6, 18.1, 19.9, 20.3, 20.9,
22.2, 22.7, 23.9, 24.8, 25.3, 25.9, 26.4, 27.0, 28.2, 28.5, 29.1, 29.7, 30.4 and 31.1 ±
0.2...