# US 8,785,455 B2 · Polymorph of linagliptin benzoate > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 8,785,455 B2 - Document ID: US8785455B2 - Status: Granted - Kind: B2 - Application number: 14/115,880 - Filed: 2012-05-09 - Published: 2014-05-01 - Granted: 2014-07-22 - Earliest claimed: 2011-05-10 - Assignees: Sandoz Ltd. - Applicants: Andreas Hotter; Arthur Pichler - Inventors: Andreas Hotter; Arthur Pichler - Web page: https://patentgrep.com/patent/US8785455B2 ## CPC - C07D 473/06: with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3 - A61K 31/522: having oxo groups directly attached to the heterocyclic ring, e.g. hypoxanthine, guanine, acyclovir - A61K 45/06: Mixtures of active ingredients without chemical characterisation, e.g. antiphlogistics and cardiaca - A61P 3/10: for hyperglycaemia, e.g. antidiabetics - A61P 43/00: Drugs for specific purposes, not provided for in groups A61P1/00-A61P41/00 - C07D 473/04: two oxygen atoms - C07D: HETEROCYCLIC COMPOUNDS (macromolecular compounds C08) - A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D) - A61P: SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS ## Abstract The present invention relates to a novel polymorph of Linagliptin benzoate and to methods for its preparation. Furthermore the present invention relates to the use of the novel polymorph for the preparation of a medicament. In addition the present invention relates to pharmaceutical compositions comprising an effective amount of the novel polymorph of Linagliptin benzoate. ## Claims ### Claim 1 A crystalline form of Linagliptin benzoate having an X-ray powder diffraction pattern comprising peaks at 2-theta angles of 8.0±0.2°, 8.7±0.2°, 10.4±0.2°, 12.9±0.2°, 13.8±0.2° and 17.4±0.2°. ### Claim 2 (depends on 1) The crystalline form of Linagliptin benzoate according to claim 1, having an infrared spectrum comprising peaks at wavenumbers of 1701±2 cm−1, 1663±2 cm−1, 1134±2 cm−1, 760±2 cm−1 and 724±2 cm−1. ### Claim 3 (depends on 1) The crystalline form of Linagliptin benzoate according to claim 1, having a DSC curve showing an endothermic peak with an onset temperature of about 193° C. ### Claim 4 (depends on 1) The crystalline form of Linagliptin benzoate according to claim 1 having a water content of about 0 w % at 3% relative humidity and about 2.0 w % at 90% relative humidity. ### Claim 5 (depends on 1) The crystalline form of Linagliptin benzoate according to claim 1 in the form of spherulitic particles, wherein the outer diameter of the spherulitic particles is from 10 to 100 μm. ### Claim 6 (depends on 1) A process for the preparation of the crystalline form of Linagliptin benzoate according to claim 1 comprising the steps of: a) dissolving Linagliptin benzoate in acetonitrile at a concentration ranging from about 10 g/l to 20 g/l upon heating; b) optionally filtering the solution; c) cooling the solution at a cooling rate of ≦−1° C./min in order to induce crystallization at a temperature above 35° C.; d) isolating the obtained crystals; and e) optionally drying the crystals. ### Claim 7 (depends on 1) A pharmaceutical composition comprising a crystalline form of Linagliptin benzoate according to claim 1, further comprising at least one pharmaceutically acceptable excipient. ### Claim 8 (depends on 7) The pharmaceutical composition according to claim 7, which is an oral dosage form. ### Claim 9 (depends on 7) The pharmaceutical composition according to claim 7 comprising additionally Metformin, Pioglitazone, a Sulfonylurea, or a pharmaceutically acceptable salt thereof. ### Claim 10 (depends on 7) The pharmaceutical composition according to claim 7 comprising additionally Metformin or a pharmaceutically acceptable salt thereof, and a Sulfonylurea or a pharmaceutically acceptable salt thereof. ### Claim 11 (depends on 1) Method of using a crystalline form of Linagliptin benzoate according to claim 1 for the preparation of a pharmaceutical composition intended for sale in a country having areas with an Af or Am climate according to the Köppen-Geiger climate classification. ### Claim 12 (depends on 1) A process for preparing a pharmaceutical composition comprising the crystalline form of Linagliptin benzoate according to claim 1, comprising the step of: mixing the crystalline form of Linagliptin benzoate according to claim 1 with at least one pharmaceutically acceptable excipient. ### Claim 13 (depends on 12) The process of claim 12, wherein mixing is effected by wet granulation. ### Claim 14 (depends on 7) A container comprising a pharmaceutical composition according to claim 7, wherein the container is prepared from a material having a permeability for water vapor as measured according to DIN 53122 of from 1.0 g*m−2*d−1 to 5000 g*m−2*d−1. ### Claim 15 (depends on 14) The container of claim 14, which is a blister package comprising an oral dosage form, wherein the blister is made from a material selected from the group consisting polyvinylchloride, polystyrole, polyamide, polyethylenevinylacetate, cellophane, celluloseacetate, and any combinations thereof. ### Claim 16 (depends on 7) The pharmaceutical composition according to claim 7, which is an oral dosage form of a capsule or tablet. ### Claim 17 (depends on 9) The pharmaceutical composition according to claim 9, which is an oral dosage form of a capsule or tablet. ### Claim 18 (depends on 10) The pharmaceutical composition according to claim 10, which is an oral dosage form of a capsule or tablet.