- Preparation and purification method of 1-(4-iodophenyl) piperidine-2,3-diketone
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The invention relates to the technical field of chemical purification, and discloses a preparation and purification method of 1-(4-iodophenyl) piperidine-2,3-dione. The method comprises the followingsteps: taking cyclopentanone oxime, and then slowly adding the cyclopentanone oxime into a chloroform suspension containing phosphorus pentachloride in a dropwise manner, wherein in the process, the temperature is controlled to be -14 DEG C to -10 DEG C; after mixing is completed, increasing the temperature to 25 DEG C, adding phosphorus oxychloride, and carrying out a reaction for 4 hours at a temperature of 60 DEG C; removing the solvent through evaporating under reduced pressure, slowly pouring the residue into crushed ice while stirring, and adjusting the pH value to be 8.1-8.5 with potassium carbonate; and stirring, and carrying out suction filtration to obtain light gray solid. According to the invention, the preparation process is clear and simple, and the preparation raw materialsare chemical raw materials which are relatively easy or commonly used on the market, so that the preparation time of a user is effectively saved, the manufacturing cost is reduced, and the environmental conditions required to be achieved in the synthesis and extraction processes are clear, simple and easy to achieve.
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Paragraph 0022-0050
(2020/06/02)
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- Apixaban intermediate and preparation method thereof
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The invention provides an apixaban intermediate and a preparation method thereof. The preparation method includes: 1) performing a bromination reaction to 5-chlorovaleryl chloride with bromine to prepare 2-bromo-5-chlorovaleryl chloride; 2) under effect o
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