- Selegiline hydrochloride synthesis process
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The invention relates to the field of chemical pharmacy, particularly to a selegiline hydrochloride preparation method. According to the invention, the method avoids the use of ephedrine, pseudoephedrine, deoxyephedrine and other management and control products, has characteristics of inexpensive and easily-available raw materials, short synthesis route, safe and environmentally-friendly production and synthesis cost reducing, can obtain the high-purity target compound at high yield, and is suitable for industrial large-scale production.
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Paragraph 0135-0141
(2020/01/25)
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- Preparation of selegiline
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A process for preparing selegiline hydrochloride by reaction of R-(-)-N,α-dimethylphenylethylamine with 3-bromo-1-propyne is described, which consists in reacting the substances in a molar ratio of approximately 2:1 at 30°-50° C. in a solvent mixture of an aromatic hydrocarbon and water and isolating the selegiline from the organic phase and converting it into the hydrochloride.
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- Improved process for the preparation of propargyl ammonium-chloride derivatives
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The present invention relates to a process for the preparation of L-isomer of propargyl-ammonium-chloride derivatives of the general formula (I) by decomposing D-tartarate of L-isomer of the amine of the general formula (II) and by reacting the obtained L-isomer amine of the general formula (II) in the presence of a base with a halide of the general formula (V), and by reacting the so-obtained L-isomer of the general formula (III) with hydrogen-chloride in an organic solvent, wherein, ???- x stands for a halogen atom,???- y stands for a hydrogen or fluorine atom, ???which comprises releasing the amine base from the D-tartarate of the L-isomer of the amine of the general formula (II), wherein y is as given above, in aqueous suspension with ammonium hydroxide or basic alkaline salt and/or ammonium salt, and reacting same with 1-1.5 mole equivalent of a halide of the general formula (V), wherein, ???- x is as defined above -, ???at 0-50 °C in a buffer system of the pH of 8-12 directly formed in the course of the base release and after separating the aqueous layer extracting the mixture containing L-isomer amines of the general formulae (II) and (III) in the organic layer with water and with a mixture of ammonium hydroxide and water and/or with a solution of aqueous phosphate salt of a pH of 5.5-7.5 and dissolving the L-isomer amine of the general formula (II) or salts thereof into the aqueous layer and selectively separating it from the L-isomer amine of the general formula (III) and converting the L-isomer amine of the general formula (III) after distillation to L-isomer salt of the general formula (I) by a method known per se.
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- Process for the preparation of propargyl ammonium-chloride
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The present invention relates to a process for the preparation of L-isomer of propargyl-ammonium-chloride derivatives of the formula (I) STR1 by decomposing D-tartarte of L-isomer of the amine of the general STR2 wherein y is hydrogen or fluoro and by reacting the obtained L-issomer amine of the formula (II) in the presence of a base with a halide of the formula (V), X--CH2 --C≡CCH wherein X is halogen and by reacting the so obtained L-isomer of the Formula (III) STR3 with hydrogen-chloride in an organic solvent, wherein x is a halogen atom, y is a hydrogen or fluorine atom.
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