Process for preparation of daclatasvir and salts
AssigneeGienmark Pharmaceuticals Limited
InventorsPrem Chand, Yogesh YADAV, Amit Anant THANEDAR, Mohammad A. KHAN, Ranjeet NAIR, Sukumar SINHA, Shekhar Bhaskar BHiRUD
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Abstract
The present invention relates to crystalline daclatasvir dihydrochloride hydrate and process for its preparation.
Claims18
Crystalline daclatasvir dihydrochloride hydrate wherein the molar ratio of daclatasvir dihydrochloride and water is in the range of 1:0.5 to 1:6.
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A process for the preparation of crystalline daclatasvir dihydrochloride hydrate, the process comprising:
- (a) dissolving daclatasvir dihydrochloride in water, optionally in the presence of a solvent, to form a solution;
- (b) heating the solution obtained in step (a) to a temperature of about 40° C. to 110° C.;
- (c) optionally maintaining the solution of step (b) at the temperature of about 40° C. to 110° C.;
- (d) cooling the solution of step (b) or step (c) to a temperature of about −5° C. to 35° C.;
- (e) isolating the crystalline daclatasvir dihydrochloride hydrate;
- and
- (f) drying the isolated crystalline daclatasvir dihydrochloride hydrate of step (e) at a temperature in the range of about 25° C. to about 60° C.
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A salt of daclatsavir with malonic acid, characterized by a proton NMR spectrum having peak positions at 11.79 (br, 2H), 7.78-7.80 (dd, 4H), 7.69-7.71 (dd, 4H), 7.55 (s, 2H), 7.31-7.33 (d, 2H), 5.08-5.10 (t, 2H), 4.08 (t, 2H), 3.8 (m, 4H) 3.54 (s, 6H), 3.2 (s, 4H), 1.95-2.17 (m, 10), 0.79-0.91 (d, 6H), 0.84-0.86 (d, 6H).
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Dependencies are inferred from the claim text.