30299-28-6Relevant articles and documents
Method for preparing high-purity kerley Bette
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, (2016/10/07)
The invention relates to a preparation method of high-purity clinofibrate, the field of preparation of pharmaceutical compounds. The preparation method comprises the following steps: reacting cyclohexanone and phenol in concentrated hydrochloric acid and glacial acetic acid in a volume ratio of 3:1-7:1 to obtain an intermediate I crude product, decolorizing with a single solvent, and cooling to crystallize to obtain an intermediate I; reacting 2-methylbutyric acid with liquid bromine in phosphorus trichloride, reacting with anhydrous alcohol, extracting, and carrying out vacuum distillation to obtain an intermediate II; reacting the intermediate I and the intermediate II under solventless conditions to obtain an intermediate III; and hydrolyzing the intermediate III and sodium hydroxide, extracting, crystallizing to obtain a clinofibrate crude product; and recrystallizing with an anhydrous solvent to obtain the clinofibrate. The material proportion is adjusted to shorten the production operation period; the invention has the advantages of low energy consumption and low solvent consumption; and the obtained product has the advantages of uniform crystal grains, high purity and low cost.