CRYSTAL COMPOUNDS Russian patent published in 2023 - IPC C07D209/52 A61K31/403 

Abstract RU 2789672 C2

FIELD: chemistry.

SUBSTANCE: invention relates to a method for the production of a monocrystal of a crystal form A of hydrochloride of (1R,5S)-1-(naphthalene-2-yl)-3-azabicyclo[3.1.0]hexane characterized by X-ray powder diffraction (hereinafter – XRPD) including values of an angle 2-theta (°), selected from a group consisting of 15.4±0.2, 16.6±0.2, 17.2±0.2, 18.5±0.2, 19.5±0.2, 20.5±0.2, 20.7±0.2, 22.9±0.2, and 25.7±0.2, where XRPD is measured using an incident bundle of CuKα radiation. The method includes stages of dissolution of hydrochloride of (1R,5S)-1-(naphthalene-2-yl)-3-azabicyclo[3.1.0]hexane in methanol; filtration through 0.2 mcm nylon filter; placement of 0.5 ml of aliquot of the filtered solution to an open vessel with a capacity of 1 drachma, which is then placed inside 20 ml vessel containing 3 ml of ethyl acetate as an antisolvent. Then, the vessel with a solution of hydrochloride of (1R,5S)-1-(naphthalene-2-yl)-3-azabicyclo[3.1.0]hexane (with a capacity of 1 drachma) is left open, and 20 ml vessel is closed, providing diffusion of vapors of both vessels; they are kept for 7 days with formation of monocrystals.

EFFECT: obtainment of a monocrystal of a crystal form A of hydrochloride of (1R,5S)-1-(naphthalene-2-yl)-3-azabicyclo[3.1.0]hexane, which is non-hygroscopic.

1 cl, 56 dwg, 21 tbl, 18 ex

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RU 2 789 672 C2

Authors

Mckinney, Anthony Alexander

Bymaster, Franklin

Piskorski, Walter

Fleitz, Fred J.

Yang, Yonglai

Engers, David A.

Smolenskaya, Valeriya

Kusukuntla, Venkat

Dates

2023-02-07Published

2016-06-17Filed