804-10-4Relevant academic research and scientific papers
Synthesis method of high-yield carbochromen bulk drug
-
Paragraph 0014; 0019-0028, (2021/08/25)
The invention relates to a high-yield synthesis method of a carbochromen bulk drug, which comprises the following steps: carrying out reflux reaction on coumarin and anhydrous potassium carbonate in a solvent, and carrying out addition reaction on coumarin and anhydrous potassium carbonate to obtain a coumarin adduct; adding the coumarin adduct into a reactor, dropwise adding an ethyl acetate hydrogen chloride saturated solution while stirring, stopping dropwise adding when the pH value of a reaction solution is equal to 6-7, performing centrifugal separation, and conducting washing with ethyl acetate; and adding isopropanol into another reactor, then adding the material washed by ethyl acetate, conducting heating and stirring until the material is completely dissolved, distilling isopropanol under normal pressure, conducting filtering and separating, and conducting refining to obtain a carbochromen finished product. The method has the advantages that the two-step method is adopted for synthesizing the detenton, the process is simple, the synthesis route is short, the reaction time is correspondingly shortened, the required reaction raw materials are few, the use of raw materials with high toxicity is avoided as much as possible, the environmental protection pressure is relieved, the final product yield is high, and the total yield can reach 34%; and the obtained carbochromen bulk drug product is high in purity, good in product quality stability and suitable for industrial production.
