Preparation method of Dabigatran etexilate key intermediate
A compound and catalyst technology, applied in the field of chemical synthesis of oral anticoagulant dabigatran etexilate intermediate, to achieve high yield, low price and low cost effect
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Embodiment 1
[0020]
[0021] Compound 2 (10.0g, 0.029mol) was added to a 250mL three-neck flask, 100mL of ethanol was added, compound 7 (5.3g, 0.032mol), ammonium chloride 1.0g, stirred and reacted at 65-70°C for 2h under nitrogen protection, the solvent was evaporated, and added Ethyl acetate 100mL, wash the organic layer with 100mL×2, wash once with saturated brine, dry over anhydrous sodium sulfate, concentrate to about 50mL, solid precipitates, add 50mL petroleum ether, stir, ice bath for one hour, filter, 50℃ 9.5 g of white solid dried under reduced pressure, yield 81%.
Embodiment 2
[0023] Compound 2 (10.0g, 0.029mol) was added to a 250mL three-necked flask, 100mL of ethanol was added, compound 7 (5.3g, 0.032mol), methanesulfonic acid 1.0g, stirred and reacted at 65-70°C for 2h under nitrogen protection, the solvent was evaporated, added Ethyl acetate 100mL, wash the organic layer with 100mL×2, wash once with saturated brine, dry over anhydrous sodium sulfate, concentrate to about 50mL, solid precipitates, add 50mL petroleum ether, stir, ice bath for one hour, filter, 50℃ 9.8 g of white solid dried under reduced pressure, yield 84%.
Embodiment 3
[0025]
[0026] Compound 2 (10.0g, 0.029mol) was added to a 250mL three-necked flask, 100mL of ethanol was added, compound 8 (7.6g, 0.032mol), ammonium chloride 1.0g, stirred and reacted at 65-70°C for 2h under nitrogen protection, the solvent was evaporated, and added Ethyl acetate 100mL, wash the organic layer with 100mL×2, wash once with saturated brine, dry over anhydrous sodium sulfate, concentrate to about 50mL, solid precipitates, add 50mL petroleum ether, stir, ice bath for one hour, filter, 50℃ 9.4 g of white solid dried under reduced pressure, yield 80%.
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