FIELD: chemistry.
SUBSTANCE: invention relates to a method for producing a crystal compound of 3-phenyl-4-propyl-1-(pyridine-2-yl)-1H-pyrazole hydrochloride. The method is carried out by a) reacting ethyl ether of 2-propyl-3-oxo-3-phenylpropionic acid with 2-hydrazinopyridine to obtain an unrefined product; b) dissolving the unrefined product in normal hexane and then slowly cooling the resulting solution to from -20 to -10°C to obtain solid substance; c) filtering, washing and drying the resulting solid substance to obtain a non-crystal compound of a free base; d) adding the non-crystal compound of a free base to a mixed solvent containing acetonitrile and distilled water in the same amount, and active mixing the resulting mixture at from 20 to 25°C to obtain crystal substance; e) filtering, washing and drying the resulting crystal substance to obtain a crystal compound of a free base, represented by the Formula 2; f) interacting of the crystal compound of a free base with a solution of hydrochloric acid – isopropyl ether to obtain solid substance of hydrochloride; g) adding solid substance of hydrochloride to a mixed solvent containing tert-butyl ether and toluene in the same amount, and active mixing the resulting mixture at from 5 to 10°C to obtain crystal substance; and h) filtering, washing and drying the resulting crystal substance to obtain a crystal compound of hydrochloride, represented by the following Formula 1.
EFFECT: technical result is the production of 3-phenyl-4-propyl-1-(pyridine-2-yl)-1H-pyrazole hydrochloride in a crystal form with stability and a lower concentration of impurities.
[Formula 2]
[Formula 1]
1 cl, 8 dwg, 5 tbl, 4 ex
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Authors
Dates
2021-08-31—Published
2018-04-20—Filed