Claims
- 1. A crystalline racemic venlafaxine base wherein said venlafaxine is in particle form having an average particle size within the range of 0.5 to 200 microns.
- 2. The venlafaxine according to claim 1, wherein said crystalline venlafaxine base has an average particle size within the range of 10 to 100 microns.
- 3. The venlafaxine according to claim 1, wherein said venlafaxine contains 2.0 wt % or less of impurities.
- 4. The venlafaxine according to claim 1, wherein said crystalline venlafaxine was formed by precipitation from a solution containing venlafaxine or a salt thereof.
- 5. The venlafaxine according to claim 1, which is substantially free of ethyl acetate.
- 6. A crystalline venlafaxine base in particle form having a bulk density of at least 0.4 mg/ml.
- 7. The crystalline venlafaxine according to claim 6, wherein said venlafaxine has a bulk density within the range of 0.4 to 0.8 mg/ml.
- 8. The venlafaxine according to claim 6, wherein said venlafaxine contains 2.0 wt % or less of impurities.
- 9. The venlafaxine according to claim 6, wherein said crystalline venlafaxine was formed by precipitation from a solution containing venlafaxine or a salt thereof.
- 10. The venlafaxine according to claim 6, which is substantially free of ethyl acetate.
- 11. A venlafaxine base in solid form and exhibiting an x-ray diffraction pattern that includes peaks at angles of 2θ of 12.8, 13.3, 18.9, and 20.0 degrees +/−0.2, said peaks having an intensity of at least 10% of the maximum intensity.
- 12. The venlafaxine according to claim 11, wherein said venlafaxine is in the form of a white powder.
- 13. The venlafaxine according to claim 11, wherein said venlafaxine is at least 98% pure.
- 14. A venlafaxine solid comprising a mixture of crystalline venlafaxine base of forms I and II.
- 15. The venlafaxine solid according to claim 14, wherein the amount of venlafaxine base of Form I comprises 80% to 99.9% of the solid.
- 16. The venlafaxine solid according to claim 14, wherein the amount of venlafaxine base of Form II comprises 80% to 99.9% of the solid.
- 17. A process for making solid racemic venlafaxine base, which comprises precipitating racemic venlafaxine base from a solution of venlafaxine to form crystalline racemic venlafaxine base; wherein said precipitation is carried out in accordance with at least one of the following conditions:
(i) said solution contains a combination of solvents comprising at least one organic polar solvent and at least one contrasolvent selected from water, an aliphatic hydrocarbon and an alicyclic hydrocarbon; or (ii) a seeding crystal of venlafaxine base is present.
- 18. The process according to claim 17, wherein said organic polar solvent is selected from the group consisting of ethyl acetate, diethyl ether, acetone, methanol, ethanol, and propanol.
- 19. The process according to claim 18, wherein said contrasolvent is selected from the group consisting of hexane, heptane, petroleum ether, and cyclohexane.
- 20. The process according to claim 17, wherein said precipitating is carried out under condition (i) and said solvent is a mixture of ethanol or ethyl acetate with n-heptane.
- 21. The process according to claim 17, wherein said precipitating is carried out under condition (i) and said solvent is a mixture of ethanol and water.
- 22. The process according to claim 17, wherein said precipitating step is carried out under condition (ii).
- 23. The process according to claim 22, wherein said seed crystal is venlafaxine Form I.
- 24. The process according to claim 22, wherein said seed crystal is venlafaxine Form II.
- 25. The process according to claim 17, wherein said precipitated venlafaxine base has an average particle size within the range of 0.5 to 200 microns and at least 50% of the particles are within the range of +/−25 microns from the average particle size.
- 26. A process for making crystalline venlafaxine base of bulk density of at least 0.4 mg/ml, which comprises crystallizing venlafaxine base from a solvent while cooling, wherein the cooling rate is not greater than 20° C./hour.
- 27. The process according to claim 26, wherein said cooling rate is about 10° C./hour.
- 28. The process according to claim 26, wherein said crystallization is carried out in the presence of a seed crystal.
Parent Case Info
[0001] This application claims the benefit of priority under 35 U.S.C. §119 from prior U.S. provisional application 60/367,736, filed Mar. 28, 2002, the entire contents of which are incorporated herein by reference.
Provisional Applications (1)
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Number |
Date |
Country |
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60367736 |
Mar 2002 |
US |