1956386-49-4Relevant academic research and scientific papers
Preparation method of penoxsulam original medicine related impurity bis-CHYMP
-
Paragraph 0029-0030; 0032-0036, (2019/03/24)
The invention provides a preparation method of penoxsulam original medicine related impurity bis-CHYMP, which comprises the following steps of: 1, dissolving 2, 4-dichloro-5-methoxy pyrimidine in methanol, adding triethylamine, adding hydrazine hydrate, carrying out reflux reaction, monitoring the reaction by TLC until the reaction is completed, cooling to room temperature, purifying to obtain 2-chlorine-5-methoxy-4-hydrazinylpyrimidine; 2, dissolving 2-chlorine-5-methoxy-4-hydroxypyrimidine in methanol, adding triethylamine, slowly dropping 2, 4-dichloro-5-methoxy pyrimidine methanol solution, carrying out reflux reaction, detecting the reaction by LCMS until the reaction is completed, cooling to obtain mixed liquid; 3, extracting, washing and concentrating the mixed liquid, preparing high performance liquid phase and purifying to obtain 2-chlorine-4-[2-(2-chlorine-5-methoxy-4-pyrimidine base) hydrazino]-5-methoxy pyrimidine; the synthetic route is shown in the description. The methodhas the advantages of economic feasibility and high yield.
