Details for Patent: 9,777,011

Title:	Process for preparing oxycodone compositions
Abstract:	In certain embodiments the invention is directed to a process for preparing an oxycodone hydrochloride composition having less than 25 ppm of 14-hydroxycodeinone.
Inventor(s):	Chapman; Robert (Downingtown, PA), Rider; Lonn S. (Foster, RI), Hong; Qi (Sharon, MA), Kyle; Donald (Yardley, PA), Kupper; Robert (East Greenwich, RI)
Assignee:	PURDUE PHARMA L.P. (Stamford, CT) THE P.F. LABORATORIES, INC. (Totowa, NJ) PURDUE PHARMACEUTICALS L.P. (Wilson, NC) RHODES TECHNOLOGIES (Coventry, RI)
Filing Date:	Mar 02, 2016
Application Number:	15/058,420
Claims:	1. A process for purifying a starting composition comprising: (a) oxycodone free base, oxycodone HCl or a mixture thereof, and (b) 14-hydroxycodeinone, comprising subjecting the composition to a hydrogenation reaction one or more times at a temperature between 40.degree. C. and 100.degree. C., wherein (i) each hydrogenation reaction is carried out for a time from 4 hours to 36 hours, and (ii) the total reaction time of all of the hydrogenation reactions is from 10 hours to 36 hours. 2. A process of claim 1, wherein the starting composition comprises oxycodone free base and 14-hydroxycodeinone. 3. The process of claim 2, wherein the starting composition further comprises 8.alpha.,14-dihydroxy-7,8-dihydrocodeinone. 4. A process of claim 3, wherein the starting composition is subjected to conditions that promote an acid catalyzed dehydration of 8.alpha.,14-dihydroxy-7,8-dihydrocodeinone to 14-hydroxycodeinone, prior to or during one or more of the hydrogenation reactions. 5. The process of claim 4, wherein 400 ppm or less of 8.alpha.,14-dihydroxy-7,8-dihydrocodeinone is present at the end of all of the hydrogenation reactions. 6. The process of claim 2, wherein at least one of the hydrogenation reactions is carried out at a temperature from 40.degree. C. to 85.degree. C. 7. The process of claim 2, wherein at least one of the hydrogenation reactions is carried out at a temperature from 75.degree. C. to 85.degree. C. 8. The process of claim 2, wherein at least one of the hydrogenation reactions is carried out for a time from 4 hours to 10 hours. 9. The process of claim 2, wherein at least one of the hydrogenation reactions is carried out for a time from 10 hours to 21.7 hours. 10. The process of claim 9, wherein the hydrogenation reaction or reactions that are carried out for a time from 10 hours to 21.7 hour are carried out at a temperature from 75.degree. C. to 85.degree. C. 11. The process of claim 2, wherein at least one of the hydrogenation reactions is carried out for a time from 21.7 hours to 36 hours. 12. The process of claim 2, wherein the hydrogenation reaction is carried out more than one time. 13. The process of claim 2, wherein less than 100 ppm of 14-hydroxycodeinone is present at the end of all of the hydrogenation reactions. 14. The process of claim 2, wherein less than 10 ppm of 14-hydroxycodeinone is present at the end of all of the hydrogenation reactions. 15. A process of claim 1, wherein the starting composition comprises oxycodone HCl and 14-hydroxycodeinone. 16. The process of claim 15, wherein the starting composition further comprises 8.alpha.,14-dihydroxy-7,8-dihydrocodeinone. 17. The process of claim 16, wherein 400 ppm or less of 8.alpha.,14-dihydroxy-7,8-dihydrocodeinone is present at the end of all of the hydrogenation reactions. 18. The process of claim 15, wherein at least one of the hydrogenation reactions is carried out at a temperature from 40.degree. C. to 85.degree. C. 19. The process of claim 15, wherein at least one of the hydrogenation reactions is carried out at a temperature from 75.degree. C. to 85.degree. C. 20. The process of claim 15, wherein at least one of the hydrogenation reactions is carried out for a time from 4 hours to 10 hours. 21. The process of claim 15, wherein at least one of the hydrogenation reactions is carried out for a time from 10 hours to 21.7 hours. 22. The process of claim 21 wherein the hydrogenation reaction or reactions that are carried out for a time from 10 hours to 21.7 hour are carried out at a temperature from 75.degree. C. to 85.degree. C. 23. The process of claim 15, wherein at least one of the hydrogenation reactions is carried out for a time from 21.7 hours to 36 hours. 24. The process of claim 15, wherein the hydrogenation reaction is carried out more than one time. 25. The process of claim 15, wherein less than 100 ppm of 14-hydroxycodeinone is present at the end of all of the hydrogenation reactions. 26. The process of claim 15, wherein less than 10 ppm of 14-hydroxycodeinone is present at the end of all of the hydrogenation reactions. 27. The process of claim 1, wherein at least 1 kg of the crystalline oxycodone HCl is prepared.