64028-40-6Relevant academic research and scientific papers
Novel synthesis process of procaterol hydrochloride
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, (2022/03/27)
The invention belongs to the technical field of medicine synthesis, and particularly relates to a synthesis process of procaterol hydrochloride. The invention provides a synthesis method of procaterol hydrochloride. The method sequentially comprises the following steps: step 1, carrying out Fries rearrangement reaction on 8-butyryloxy quinolone and butyryl chloride to obtain a mixture; 2, directly reacting the mixture obtained in the step 1 with a benzyl compound and alkali to obtain a mixture; step 3, enabling the mixture obtained in the step 2 to react with pyridinium tribromide in tetrahydrofuran to obtain 5-(2-bromobutyryl)-8-benzyloxy quinolone; step 4, carrying out ammonolysis reaction on the product in the step 3 and isopropylamine in tetrahydrofuran; 5, the product in the step 4 is subjected to a reduction reaction in an alcohol solvent, and 5-(2-isopropylamine-1-hydroxybutyl)-8-benzyloxy quinolone is obtained; and 6, carrying out hydrogenation reduction reaction on the product obtained in the step 5 under the catalysis of a catalyst, and carrying out salt forming reaction with hydrochloric acid to obtain procaterol hydrochloride.
Procaterol hydrochloride impurity preparation method
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Paragraph 0029-0031, (2021/04/14)
The invention discloses a procaterol hydrochloride impurity preparation method, which comprises: 1, adding procaterol hydrochloride to an organic solvent under an alkaline condition, adding an appropriate amount of benzyl halide, carrying out heating reflux until the reaction is complete, and carrying out post-treatment to obtain an intermediate 1; step 2, adding the intermediate 1 into a reaction bottle, then adding an organic solvent, raising the temperature, adding an oxidant aqueous solution, pouring into ice water after heating reaction is completed, and separating out a solid to obtain an intermediate 2; and step 3, adding the intermediate 2 into a reaction bottle, then adding an organic solvent, cooling to a low temperature, slowly adding boron trichloride, keeping the low temperature until the reaction is complete, pouring into ice water, separating out solids, and filtering to obtain the procaterol impurity. Procaterol hydrochloride which is easy to obtain is used as an initial raw material to prepare the procaterol hydrochloride impurity, the synthesis cost of the procaterol hydrochloride impurity is reduced, the preparation steps of the procaterol hydrochloride impurity are simplified, and the selectivity is improved, so that the preparation time is saved, and the preparation efficiency is improved. The total yield of the reaction is 50-70%.
