US 10,538,507 B2 · Preparation process for high-purity dabigatran etexilate

Abstract

Provided is a purifying method for dabigatran etexilate free base, comprising subjecting a dabigatran etexilate free base crude product to water slurrying to obtain a crude product B; then conducting recrystallization on the crude product B with acetone and water to obtain a crude product C; and subsequently, purifying the crude product C with a mixed solvent of tetrahydrofuran and ethyl acetate, filtering and drying to obtain a dabigatran etexilate free base finished product. The purifying method of the present invention can effectively remove various impurities and is suitable for workshop production. Salts and water-soluble organic impurities are removed by purified water slurrying, impurities with a high polarity are removed by purifying with an acetone-water solution, and impurities with a low polarity are removed by purifying with a mixed solvent of tetrahydrofuran and ethyl acetate.

Claims8

Dependent claims

A process for the preparation of high-purity dabigatran etexilate comprising:

a) adding a crude product of dabigatran etexilate into water, slurrying at 5-30° C., and filtering after slurrying for 1-2 h to get a crude product B;
b) adding the crude product B into acetone, heating up to 20-50° C. to obtain a clear solution, then adding water dropwise into the solution, cooling the solution to 0-10° C., and filtering to get a crude product C;
and
c) adding the crude product C into a mixture of tetrahydrofuran and ethyl acetate, heating up to 50-70° C. to dissolve, and then cooling to 40-45° C., slowly cooling to 0-5° C., then filtering, drying filter cake at 40-50° C. under vacuum to obtain the high-purity dabigatran etexilate.

1 more element

Dependencies are inferred from the claim text.

Preparation process for high-purity dabigatran etexilate

Life of this patent

Preparation process for high-purity dabigatran etexilate

Life of this patent

Abstract

Claims8