A new preparation process of azilsartan
A technology of compound and synthesis method, which is applied in the field of medicine and chemical industry, can solve the problems of long steps and limitations of industrial production, and achieve the effect of less by-products, short method route and mild reaction conditions
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Embodiment 1
[0020] The synthesis of embodiment 1. compound 3:
[0021] Compound 1 (7.4g, 40mmol), compound 2 (5.9g, 40mmol), Na 2 CO 3 (2M, 80 mmol, ), Pd(dppf)Cl 2 (2mmol) and 150mL of ethylene glycol dimethyl ether were added successively in a 500mL flask under a nitrogen atmosphere, refluxed for 2 hours, then extracted with ethyl acetate, NaHCO3 solution, brine were washed successively, dried over anhydrous magnesium sulfate, filtered, The crude product obtained by concentration was directly used in the next step without purification.
Embodiment 2
[0022] The synthesis of embodiment 2. compound 5:
[0023] Compound 4 (9.0g, 41mmol), Na 2 CO 3 (8.7g, 82mmol), compound 3 (8.1g, crude product) and 150mL of DMF were added to a 250mL flask, reacted at 130°C for 2h, cooled, concentrated, diluted with water, extracted with ethyl acetate, dried, and purified by column chromatography 5 (13g, yield, 80%)
Embodiment 3
[0024] The synthesis of embodiment 3. compound 6:
[0025] SnCl 2 (10g, 54mmol) was added in the ethyl acetate (300mL) solution of compound 5 (13g, 32mmol), then refluxed for 17h, after monitoring that the reaction was complete, direct concentration column chromatography purified to obtain compound 6 (10.5g, yield 87%)
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