SYNTHESIS OF 1-AMINO-1,3,3,5,5-PENTAMETHYLCYCLOHEXANE MESYLATE Russian patent published in 2014 - IPC C07C211/35 C07C303/32 C07C309/04 C07C211/62 A61K31/13 A61K31/14 A61P25/28 

FIELD: chemistry.

SUBSTANCE: claimed compound can be used in case of diseases and states, such as tinnitus, neuropathic pain and in treatment of Alzheimer's diseases. Method includes stage (1): interaction of 1-amino-1,3,3,5,5-pentamethylcyclohexane with methanesulfonic acid in anisole at temperature from 50°C to 100°C and ratio of anisole volume to weight of 1-amino-1,3,3,5,5-pentamethylcyclohexane from 5 to 15 ml of anisole per gram of 1-amino-1,3,3,5,5-pentamethylcyclohexane. Solvent can contain dissolved in it water. Metod can also include stage (ii): separation of 1-amino-1,3,3,5,5-pentamethylcyclohexane mesylate from reaction mixture of stage (i) by crystallisation with decrease of temperature in the range from -20°C to 50°C. Additionally, after stage (i) or stage (ii), method can include at least one of stages (iii)-(v). Stage (iii) consists in recrystallisation of product, formed at stage (i) or stage (ii) from anisole; stage (iv) includes addition of 1-amino-1,3,3,5,5-pentamethylcyclohexane mesylate at any of preceding stages (i)-(iii); and stage (v) ingludes deagglomeration and/or crushing product, formed at any of preceding stages (i)-(iv). Crystals, obtained at stage (iv) are star-shaped. At stage (ii) or at stage (iv) also obtained are particles of 1-amino-1,3,3,5,5-pentamethylcyclohexane mesylate, where less than 15% in weight of particles have particle size 10 mcm and less or where less than 10% in weight of particles have particle size 10 mcm and less. Before separation of 1-amino-1,3,3,5,5-pentamethylcyclohexane mesylate, mixture, obtained at stage (i), (ii) or (iii), is usually cooled to room temperature or below room temperature at rate of cooling from 0.05°C/min to 2°C/min.

EFFECT: invention relates to improved method of obtaining 1-amino-1,3,3,5,5-pentamethylcyclohexane mesylate.

11 cl, 6 dwg, 2 tbl, 22 ex