- Preparation method of vildagliptin cyclic amidine impurity
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The invention discloses a preparation method of a vildagliptin cyclic amidine impurity. The preparation method comprises the following steps: adding a reaction solvent into vildagliptin (I) and addingalkali; raising the temperature to 30 to 180 DEG C, wherein the reaction time is 2 to 8h; purifying a reaction solution to obtain the vildagliptin cyclic amidine impurity (II). The invention providesa synthesis method of the vildagliptin cyclic amidine impurity for the first time; the vildagliptin is used as a raw material and the vildagliptin cyclic amidine impurity is prepared by adopting one-step ring-forming reaction; the preparation method is moderate in reaction conditions, is easy to operate and high in yield. A product, which accords with quality standards, can be obtained through simple purification and the research and development cost is effectively reduced.
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Paragraph 0024; 0025; 0026; 0027; 0028; 0029; 0030-0035
(2018/08/28)
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- The preparation method of the peculiar smell degradation impurity
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The invention discloses a method for preparing vildagliptin degraded impurities 2-(3-hydroxyl-adamantine-1-yl)-1-imido-hexahydro pyrrolo[1, 2-a] pyrazine-4-one and 2-(3-hydroxyl-adamantine-1-yl)-hexahydropyrrolo[1, 2-a] pyrazine-1, 4-dione. The method comprises the following steps: performing high-temperature degrading and performing column chromatography isolation by taking the vildagliptin as the starting material to obtain the 2-(3-hydroxyl-adamantine-1-yl)-1-imido-hexahydro pyrrolo[1, 2-a] pyrazine-4-one, and reacting with water and performing column separation to obtain the 2-(3-hydroxyl-adamantine-1-yl)-hexahydropyrrolo[1, 2-a] pyrazine-1, 4-dione. The method has the beneficial effects of preparing the standard substances of the vildagliptin degraded impurities 2-(3-hydroxyl-adamantine-1-yl)-1-imido-hexahydro pyrrolo[1, 2-a] pyrazine-4-one and 2-(3-hydroxyl-adamantine-1-yl)-hexahydropyrrolo[1, 2-a] pyrazine-1, 4-dione with the purity of more than 97%.
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Paragraph 0058; 0060; 0073-0078; 0089-0096
(2017/10/07)
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- Preparation method of degrading impurities by means of vildagliptin
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The invention relates to the technical field of chemical industry, and discloses a preparation method of degrading impurities by means of vildagliptin. The preparation method comprises the steps that vildagliptin, a first compound and a second compound react to generate N-(3-hydroxyl adamantane)-1-imino-hexahydro-pyrrole[1,2-a]pyrazine-4(1H)-one, wherein the first compound is ethyl acetate or methylbenzene, and the second compound is triethylamine or diisopropylethylamine. According to the preparation method of degrading the impurities by means of vildagliptin, vildagliptin serves as the raw material, appropriate reactants are selected for preparing degradation products of vildagliptin, the technology is simple and convenient, the yield and purity are high, and a basis is provided for controlling the quality standard of pharmaceutical products of vildagliptin.
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Paragraph 0032; 0033; 0034; 0035; 0036; 0037-0054; 0064
(2017/07/19)
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