- Method for synthesizing lorcaserin intermediate p-chlorophenethylamine
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The invention discloses a method for synthesizing a lorcaserin intermediate, namely p-chlorophenethylamine. The method is characterized in that p-chlorophenethylamine is prepared from p-halogen chlorobenzene and halogenated ethylamine under the action of a catalyst, and the reaction process comprises the following steps: 1) uniformly mixing halogenated ethylamine, a protecting agent, an alkali 1 and a solvent S1, stirring at 50-70 DEG C to perform a reaction for 6-8h, and filtering off solids so as to obtain a mixture M1; 2) under the protection of a protection gas, uniformly mixing p-halogenchlorobenzene, copper iodide, a solid alkali and a solvent S2, controlling a reaction temperature to 130-145 DEG C and reaction pressure to 3-5atm, stirring for 50-70min, dropping the mixture M1, controlling the reaction temperature to 150-170 DEG C and the reaction pressure to 5-7atm after dropping is completed, and carrying out a reaction for 1-2 so as to obtain a mixture M2; 3) putting a hydrochloric acid solution into the mixture M2, controlling the reaction temperature to 80-90 DEG C and t he reaction pressure to 2-3atm, and carrying out a reaction for 40-60min so as to obtain a mixture M3; and 4) putting an alkali 2 into the mixture M3 to adjust the pH value to 4, controlling the temperature to be less than 70 DEG C, cooling, leaving to stand and layer, washing an organic phase withwater, drying with a drying agent, and concentrating and evaporating off the solvents, thereby obtaining a product. The method is simple in operation, and no toxic substance is used.
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Page/Page column 0031; 0034; 0035; 0036
(2019/09/13)
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- Deacetylative Amination of Acetyl Arenes and Alkanes with C-C Bond Cleavage
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The Br?nsted acid-catalyzed synthesis of primary amines from acetyl arenes and alkanes with C-C bond cleavage is described. Although the conversion from an acetyl group to amine has traditionally required multiple steps, the method described herein, which uses an oxime reagent as an amino group source, achieves the transformation directly via domino transoximation/Beckmann rearrangement/Pinner reaction. The method was also applied to the synthesis of γ-aminobutyric acids, such as baclophen and rolipram.
- Hyodo, Kengo,Hasegawa, Genna,Maki, Hiroya,Uchida, Kingo
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p. 2818 - 2822
(2019/04/25)
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- Preparation method and use of lorcaserin hydrochloride
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The invention provides a preparation method of lorcaserin hydrochloride, wherein the preparation method comprises the synthetic route described in the specification. The preparation method of lorcaserin hydrochloride has the advantages of simpliness, cheap and easily available raw materials, convenient and safe post-processing, and more green and environmental-protection preparation process, and is an economic synthetic method which can be industrialized.
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Paragraph 0019; 0020
(2017/08/28)
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- Preparation method of lorcaserin hydrochloride
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The invention relates to the field of medicinal chemistry, and specifically discloses a preparation method of lorcaserin hydrochloride namely (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride. The preparation method is characterized in that 4-chlorophenethylamine as a raw material is successively subjected to acylation and amino protection, allyl substitution, Friedel-Crafts alkylation, resolution and salifying to obtain lorcaserin hydrochloride. The preparation method of lorcaserin hydrochloride has the advantages of high yield, low cost, simple operation and the like, and is an economic and industrializable synthesis method.
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Paragraph 0040; 0041; 0042
(2017/01/09)
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- A kind of products and intermediates green card color forest hydrochloride method for the preparation of (by machine translation)
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The invention relates to the field of pharmaceutical chemistry, in particular relates to a diet green card color forest hydrochloride method for the preparation of intermediates thereof. The utility model is characterized in that the preparation method comprises: to the chlorobenzene ethylamine as raw materials, after sequentially acidylated protecting amino group, allyl substituted, deprotected, gram alkylate tougheness, split, a green card color forest of the hydrochloric acid salt. green card color forest hydrochloric acid of the present invention and wherein the intermediate preparation method is low in cost, simple in operation, after treatment is convenient, is an economical, can be industrial synthetic method. (by machine translation)
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Paragraph 0047; 0048; 0049
(2016/10/07)
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- Novel Synthesis of Antiobesity Drug Lorcaserin Hydrochloride
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A novel synthesis of antiobesity drug lorcaserin hydrochloride was accomplished in six steps. N-protection of 2-(4-chlorophenyl)ethanamine with di-tert-butyl dicarbonate, N-alkylation with allyl bromide, deprotection, intramolecular Friedel-Crafts alkylation, chiral resolution with l-(+)-tartaric acid, and the final salification led to the target molecule lorcaserin hydrochloride in 23.1% overall yield with 99.9% purity and excellent enantioselectivity (>99.8% ee). This convenient and economical procedure is remarkably applicable for scale-up production.
- Zhu, Qihua,Wang, Junwei,Bian, Xueguo,Zhang, Lingzhi,Wei, Ping,Xu, Yungen
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p. 1263 - 1267
(2015/09/28)
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- PROCESS FOR THE ENANTIOSELECTIVE SYNTHESIS OF A TETRAHYDROBENZAZEPINE COMPOUND
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This invention relates to an improved process for the enantioselective synthesis of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine
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Paragraph 0091
(2014/05/07)
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