IP Library Granted Patent US 7,067,546
Granted Patent B2
US 7,067,546 · App. 10/485,593 · Granted Jun 27, 2006

Crystal and process for producing the same

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Quick Facts
Patent No.
US 7,067,546
App. No.
10/485,593
Granted
Jun 27, 2006
Kind
B2
Abstract

A process for producing crystals of 2-ethoxy-1-[[2′-(1H-tetrazol-5-yl) biphenyl-4-yl]methyl]-1H-benzimdazole-7-carboxylic acid (compound (I)), characterized by dissolving or suspending the compound (I) or a salt thereof in a solvent comprising an aprotic polar solvent and crystallizing it. By the process, the contaminants which are contained in the compound (I) or its salt and are difficult to remove, such as tin compounds, analogues of the compound (I), and a residual organic solvent, can be easily removed. Crystals of the compound (I) can be efficiently and easily mass-produced in high yield on an industrial scale.

Claims (10)

1. A process for producing a crystal of 2-ethoxy-1-[[2′-(1H-tetrazol-5-yl)biphenyl-4-yl]methyl]-1H-benzimidazole-7-carboxylic acid, which comprises crystallizing from a solution or suspension containing 2-ethoxy-1-[[2′-(1H-tetrazol5-yl) biphenyl-4-yl]methyl]-1H-benzimidazole-7-carboxylic acid or a salt thereof and an aprotic polar solvent, wherein the aprotic polar solvent is tetrahydrofuran, dimethylformamide, dimethyl sulfoxide, hexamethylphosphoric triamide, or a mixed solvent of two or more of them.

2. A process for producing a crystal of 2-ethoxy-1-[[2′-(1H-tetrazol-5-yl) biphenyl-4-yl]methyl]-1H-benzimidazole-7-carboxylic acid, which comprises crystallizing from a solution containing 2-ethoxy-1-[[2′-(1H-tetrazol-5-yl)biphenyl-4-yl]methyl]-1H-benzimidazole-7-carboxylic acid and an aprotic polar solvent, wherein the aprotic polar solvent is tetrahydrofuran, dimethylformamide, dimethyl sulfoxide, hexamethylphosphoric triamide, or a mixed solvent of two or more of them.

3. The process according to claim 1 wherein the aprotic polar solvent is one or more kinds of solvents selected from tetrahydrofuran, dimethylformamide, dimethyl sulfoxide and hexamethylphosphoric triamide.

4. The process according to claim 1 wherein the aprotic polar solvent is tetrahydrofuran.

5. The process according to claim 1 which comprises crystallizing at about 0 to about 30° C.

6. The process according to claim 1 wherein a step in which a crystallized crystal is dissolved or suspended in a solvent containing an aprotic polar solvent, followed by being crystallized, is repeated one or more times.

7. The process according to claim 2 wherein the aprotic polar solvent is one or more kinds of solvents selected from tetrahydrofuran, dimethylformamide, dimethyl sulfoxide and hexamethylphosphoric triamide.

8. The process according to claim 2 wherein the aprotic polar solvent is tetrahydrofuran.

9. The process according to claim 2 which comprises crystallizing at about 0 to about 30° C.

10. The process according to claim 2 wherein a step in which a crystallized crystal is dissolved or suspended in a solvent containing an aprotic polar solvent, followed by being crystallized, is repeated one or more times.

Assignments (2)
CHANGE OF NAME Recorded May 16, 2005
From: TAKEDA CHEMICAL INDUSTRIES, LTD.
To: TAKEDA PHARMACEUTICAL COMPANY LIMITED
Reel/Frame 016891/0046 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 2, 2004
From: HASHIMOTO, HIDEO; MARUYAMA, HIDEAKI
To: TAKEDA CHEMICAL INDUSTRIES LTD.
Reel/Frame 015504/0277 →