7531-52-4Relevant articles and documents
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Takahashi,Cohen
, p. 864,865 (1969)
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Preparation method of L-prolinamide
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Paragraph 0039; 0041-0048, (2021/01/28)
The invention provides a preparation method of L-prolinamide. The preparation method comprises the following steps: by using L-proline as an initial raw material, firstly forming L-proline methyl ester hydrochloride, then carrying out ammonolysis to obtain a synthetic solution containing L-prolinamide, and dissociating the residual L-prolinamide hydrochloride in the synthetic solution into L-prolinamide through inorganic alkali in a non-aqueous environment, and removing by-products through a non-aqueous solvent system. According to the preparation method, the L-prolinamide hydrochloride can befully dissociated, the by-products and the impurities can be effectively removed, the yield and purity of the target product can be remarkably improved, the preparation method is simple and convenient in process, mild in condition and easy to control, expensive reagents are not needed, the production efficiency of the L-prolinamide can be improved, and the preparation method is suitable for large-scale industrial production and has important economic and social values.
Synthesis method of L-prolinamide
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Paragraph 0030; 0034; 0035; 0039; 0040; 0044; 0045; 0049, (2019/01/16)
The invention belongs to the field of organic synthesis, and discloses a synthesis method of L-prolinamide. The method comprises steps of S1, dissolving an initial material, L-proline, in water and then reacting with acetic anhydride, after reaction, extracting and drying to prepare N-acetyl-L-proline; S2, in a solvent system, performing a reaction on a raw material, N-acetyl-L-proline prepared inS1 and thionyl chloride, then concentrating and drying to obtain a compound; S3, dripping aqueous ammonia in the compound prepared in S2 as a raw material so as to react, filtering and preparing 1-acetyl-2-pyrrolidinecarboxamide; and S4, dripping HC1 into the 1-acetyl-2-pyrrolidinecarboxamide prepared in S3 as a raw material, so as to react, then concentrating, filtering and drying to prepare L-prolinamide. In the reaction process of the synthesis method provided by the invention, common reagent raw materials are used, the costs are low, the reaction conditions are mild, the chiral purity ishigh, the yield is high, the environment pressure is low, and the synthesis method is suitable for large-scale production.
Synthesis method of L-prolinamide
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Paragraph 0023; 0024; 0025, (2018/03/26)
The invention relates to the technical field of medicines, in particular to a synthesis method of L-prolinamide. The synthesis method comprises the steps of (1) dissolving the L-prolinamide into an alcoholic solution, adding an esterification reagent for reacting, and obtaining an intermediate product II; (2) adding the product II of the step (1) into an alcoholic solution of ammonia, transferringto a high pressure reactor, and carrying out ammonia-feeding reaction; (3) decompressing and concentrating a reaction liquid in the step (2), and filtering to obtain a primary filter liquor; (4) desalinizing the primary filter liquor in the step (3), and filtering to obtain a secondary filter liquor; (5) decompressing and concentrating the secondary filter liquor of the step (4), adding a solventfor dissolving and crystalizing, cooling for suction filtration, and obtaining a product I. The synthesis method provided by the invention is simple to operate, less in waste water and waste gas, clean and environmentally-friendly. The total yield of the L-prolinamide is 78 percent, the product HPLC (High Performance Liquid Chromatography) purity is 99.6 percent, the maximum individual impurity is less than or equal to 0.3 percent, and a D type isomer is less than or equal to 0.3 percent.