455-03-8Relevant articles and documents
Preparation method of cinacalcet hydrochloride
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Paragraph 0036; 0038; 0040, (2020/10/05)
The invention provides a preparation method of cinacalcet hydrochloride, which comprises the following steps: (1) reacting a compound as shown in a formula I with thionyl chloride under the conditionsthat isopropyl acetate and N, N-dimethylformamide are used as solvents and the temperature is 40-45 DEG C to obtain a product; (2) directly reacting the product obtained in the step (1) with a raw material A to obtain an intermediate I; and (3) carrying out reduction reaction and refining on the intermediate I obtained in the step (2) to obtain cinacalcet hydrochloride. According to the preparation method provided by the invention, by using isopropyl acetate and N, N-dimethylformamide (DMF) as solvents in the first-step reaction, compared with the prior art requiring the reaction conditions of higher reaction temperature and a large amount of thionyl chloride, the temperature is greatly reduced, the use amount of thionyl chloride is reduced, higher yield is still ensured, and the method has higher industrialization value.
Method for synthesizing cinacalcet hydrochloride intermediate in microchannel reactor
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Paragraph 0065-0081; 0087-0089, (2019/11/12)
The invention provides a method for synthesizing cinacalcet hydrochloride intermediate in a microchannel reactor. The method comprises the steps that 3-(3-trifluoromethylphenyl)-2-acrylic acid and a supported noble metal catalyst are added into an organic solvent A to react with hydrogen to generate 3-(3-trifluoromethylphenyl)propionic acid; after the reaction, filtration is conducted, and a catalyst B and thionyl chloride are added into filtrate to react to generate 3-(3-trifluoromethylphenyl)propionyl chloride, and the two intermediates are all finished in the microchannel reactor. By usingefficient mass transfer and heat transfer of the microchannel reactor, time of hydrogenation is effectively shortened, generation of esterification by-products in the hydrogenation process is prevented, the purity and yield of products are improved, palladium carbon is recovered and applied ,mechanically for many times, cumbersome operation in the kettle reaction process is overcome, and at the same time, materials generated in the reaction can be directly used for the next reaction; and the usage amount of the thionyl chloride in the preparation process of acyl chloride is reduced, waste discharge is reduced, and a green process for synthesizing cinacalcet hydrochloride intermediate is provided.
Rh(III)-Catalyzed meta-C-H Olefination Directed by a Nitrile Template
Xu, Hua-Jin,Lu, Yi,Farmer, Marcus E.,Wang, Huai-Wei,Zhao, Dan,Kang, Yan-Shang,Sun, Wei-Yin,Yu, Jin-Quan
supporting information, p. 2200 - 2203 (2017/02/23)
A range of Rh(III)-catalyzed ortho-C-H functionalizations have been developed; however, extension of this reactivity to remote C-H functionalizations through large-ring rhodacyclic intermediates has yet to be demonstrated. Herein we report the first examp