Preparation method of Dabigatran etexilate key intermediate
A compound and catalyst technology, applied in the field of chemical synthesis of oral anticoagulant dabigatran etexilate intermediates, can solve the problems of unsuitability for industrial production, increase of production cost, high preparation cost, etc., and achieve short reaction time and high yield The effect of low cost and convenient purification
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[0017] Example 1
[0018]
[0019] Compound 2 (10.0 g, 0.029 mol) was added to a 250 mL three-necked flask, 100 mL of ethanol was added, compound 7 (5.3 g, 0.032 mol), ammonium chloride 1.0 g, and the reaction was stirred at 65-70 °C for 2 h under nitrogen protection. 100 mL of ethyl acetate, washed the organic layer with 100 mL × 2, washed with saturated brine once, dried over anhydrous sodium sulfate, concentrated to about 50 mL, a solid was precipitated, added 50 mL of petroleum ether, stirred, ice bathed for one hour, filtered, 50 ° C The white solid dried under reduced pressure was 9.5 g, and the yield was 81%.
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[0020] Example 2
[0021] Compound 2 (10.0 g, 0.029 mol) was added to a 250 mL three-necked flask, 100 mL of ethanol was added, compound 7 (5.3 g, 0.032 mol), methanesulfonic acid 1.0 g, and the reaction was stirred at 65-70 °C for 2 h under nitrogen protection. 100 mL of ethyl acetate, washed the organic layer with 100 mL × 2, washed with saturated brine once, dried over anhydrous sodium sulfate, concentrated to about 50 mL, a solid was precipitated, added 50 mL of petroleum ether, stirred, ice bathed for one hour, filtered, 50 ° C The white solid dried under reduced pressure was 9.8 g, and the yield was 84%.
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[0022] Example 3
[0023]
[0024] Compound 2 (10.0 g, 0.029 mol) was added to a 250 mL three-necked flask, 100 mL of ethanol was added, compound 8 (7.6 g, 0.032 mol), ammonium chloride 1.0 g, and the reaction was stirred at 65-70 °C for 2 h under nitrogen protection. 100 mL of ethyl acetate, washed the organic layer with 100 mL × 2, washed with saturated brine once, dried over anhydrous sodium sulfate, concentrated to about 50 mL, a solid was precipitated, added 50 mL of petroleum ether, stirred, ice bathed for one hour, filtered, 50 ° C The white solid dried under reduced pressure was 9.4 g, and the yield was 80%.
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