26646-51-5Relevant academic research and scientific papers
Preparation method of roxatidine acetate hydrochloride
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Paragraph 0052; 0083-0085; 0097-0099; 0111-0113, (2020/05/01)
The invention relates to a preparation method of roxatidine acetate hydrochloride. The preparation method comprises the following steps: step 1, dissolving m-cresol and 3-chloropropylamine hydrochloride into a reaction solvent according to a certain ratio, carrying out a reaction in the presence of an alkali, extracting after the reaction, and concentrating after simple purification to obtain an intermediate 1; 2, dissolving the intermediate 1 and an alkali in a reaction solvent according to a certain ratio, adding acetoxyacetyl chloride in a dropwise manner at a low temperature, and extracting and concentrating after the reaction of the intermediate 1 is finished to obtain an intermediate 2; 3, carrying out a bromination reaction on the intermediate 2 and N-bromosuccinimide, and directlycarrying out water washing extraction to obtain an intermediate 3; 4, carrying out a reaction on the intermediate 3 and excessive piperidine in a solvent, concentrating, extracting with dichloromethane, drying, and further purifying with acetic anhydride to obtain roxatidine acetate; 5, dissolving the intermediate 3 in acetone, adding hydrochloric acid in a dropwise manner to form a salt, filtering, and drying; and 6, mixing with absolute ethyl alcohol, filtering, carrying out cooling crystallization, and drying to obtain the roxatidine acetate hydrochloride.
