Preparation method of telmisartan
A technology for telmisartan and coupling reaction, which is applied in a preparation field of telmisartan, can solve the problems of low yield, high temperature, unfavorable industrial production, etc., and achieves high reaction yield, mild reaction conditions, and low cost. The effect of advantage
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Embodiment 1
[0021] Synthesis of Telmisartan
[0022] Add 4.2g of compound 3 to 50ml of dioxane, then add 2.2g of compound 2, 3.8g of sodium carbonate and 0.2g of palladium acetate, fill with nitrogen, heat to 80°C, stir for 6 hours, and monitor the reaction by spotting complete, cooled to room temperature, filtered, the filtrate was concentrated, the residue was passed through a flash column, and the eluate was concentrated and then recrystallized with ethyl acetate, filtered and dried to obtain 4.59g of the product telmisartan as a white crystalline powder with a yield of 90.05%. The HPLC purity is 99.8%, and the single impurity is less than 0.1%.
Embodiment 2
[0024] Synthesis of Telmisartan
[0025] Add 4.2g of compound 3 to 50ml of toluene respectively, then add 2.2g of compound 2, 4.2g of potassium carbonate and 0.2g of palladium acetate, fill with nitrogen, heat to 80°C, stir and react for 6.5 hours, spot the plate to monitor the reaction is complete, cool to room temperature, filtered, the filtrate was concentrated, the residue was passed through a flash column, and the eluent was concentrated and then recrystallized with ethyl acetate, filtered, and dried to obtain 4.46g of product telmisartan as a white crystalline powder, with a yield of 87.4% and a HPLC purity of 99.7 %, a single impurity is less than 0.1%.
Embodiment 3
[0027] Synthesis of Telmisartan
[0028] Add 4.2g of compound 3 to 50ml of N,N-dimethylformamide, then add 2.2g of compound 2, 4.2g of potassium carbonate and 0.2g of palladium chloride, fill with nitrogen, heat to 80°C, and stir for 8 Hours, spot plate monitoring reaction is complete, cool to room temperature, filter, the filtrate is concentrated, and the residue is passed through a flash column. After the eluate is concentrated, it is recrystallized with ethyl acetate, filtered, and dried to obtain 4.31g of product telmisartan as a white crystalline powder , yield 85.2%, HPLC purity 99.5%, single impurity less than 0.1%.
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