反应详情

温度

10 °C

350 mL acetone, 250 mL water and 32.2 g potassium carbonate were stirred in round bottom flask at 25° C. The reaction mixture was cooled to 10° C. and 100 g of 1-methyl-2-[N-(4-amidinophenyl)aminomethyl]benzimidazol-5-yl-carboxylic acid-N-phenyl-N-(2-ethoxy carbonylethyl)amide hydrochloride of Formula (E) was added. 15 mL acetone and 16.8 mL n-hexyl chloroformate were added to the reaction mixture and stirred for 1 hour. The precipitated product was filtered and washed with mixture of acetone and water. The wet-cake was dissolved in acetone and stirred for 30 min. The product was obtained by addition of water followed by filtration. The wet-cake thus obtained was washed with acetone and dried to obtain dabigatran etexilate of Formula (E). 50 g dabigatran etexilate and 500 mL ethyl acetate were stirred at 25° C. The reaction mixture was charcoalized and filtered. The filtrate was heated 75° C. to 80° C. and stirred for 30 minutes and cooled to 25° C. to 35° C. The reaction mixture was filtered and washed with ethyl acetate to obtain pure dabigatran etexilate of Formula (F).

1. filtrationThe precipitated product was filtered
2. washwashed with mixture of acetone and water
3. dissolutionThe wet-cake was dissolved in acetone
4. stirringstirred for 30 min
5. customThe product was obtained by addition of water
6. filtrationfollowed by filtration
7. customThe wet-cake thus obtained
8. washwas washed with acetone
9. customdried