- Preparation method of aliskiren intermediate
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The invention relates to a preparation method of an important intermediate trans-(2S)-5-chloro-2-isopropyl-N, N-dimethyl-4-pentanamide for synthesizing aliskiren. The method comprises the following steps: by taking trans-(2S)-5-chloro-2-isopropyl-N, N-dimethyl-4-pentanamide as a raw material and dichloromethane as a solvent, reacting trans-(2S)-5-chloro-2-isopropyl-4-pentenoic acid with 2-chloro-4, 6-dimethoxy-1, 3, 5-triazine under the action of an organic alkali, then reacting with dimethylamine hydrochloride, and carrying out acid washing, alkali washing, drying and reduced pressure distillation to obtain the high-purity target intermediate. According to the method, a one-pot method is adopted, and an acyl chloride intermediate is not separated in the process, so that the risk of chiral carbon racemization of trans-(2S)-5-chloro-2-isopropyl-4-pentenoyl chloride in the reaction and high-temperature distillation processes under a high-temperature acidic condition and the decomposition of acyl chloride in the separation process are avoided, and the purity and yield of a target product are improved; and operation is simple and convenient, the same solvent is adopted in the whole synthesis process, a large amount of organic solvent is saved, the production cost is low, the production efficiency is high, and the method is more suitable for industrial production.
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Paragraph 0033; 0035-0038; 0040-0043; 0045-0047
(2021/09/15)
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- A aliskiren or its salt separation and analysis method
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The invention relates to a separation analysis method using polysaccharide derivative-bonded and coated silica as a stationary phase and an organic solvent as a mobile phase for separation analysis of aliskiren and isomers thereof, effective separation of the aliskiren and isomers thereof can be realized, and the separation analysis method has the important meaning to the product quality control.
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- PROCESS FOR PREPARING ALISKIREN AND ITS INTERMEDIATES
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The present application relates to a process for the preparation of aliskiren and its pharmaceutically acceptable salts. In particular, the present application relates to a process for the preparation of intermediates for aliskiren, and their conversion to aliskiren or its salts.
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- 2-ALKYL-5-HALOGEN-PENT-4-ENE CARBOXYLIC ACIDS AND THEIR PRODUCTION
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From compounds of formula II wherein R1 and R2 are independently of one another H, C1-C6alkyl, C1-C6halogenalkyl, C1-C6alkoxy, C1-C6alkoxy-C
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