反応 #644337

反応方程式

hydrochloric acid

Oxycodone

14-hydroxycodeinone

water

→

oxycodone hydrochloride

溶媒

1-butanol

反応条件

後処理

1. 1
   その他At 15° C. and with the reaction under nitrogen
2. 2
   workup.ADDITIONActivated carbon (Norit KB-G, 4 g) was added to the reactor
3. 3
   workup.STIRRINGto stir for 40 min
4. 4
   ろ過The reaction mixture was then filtered
5. 5
   その他to remove the zinc and carbon
6. 6
   workup.ADDITIONThe filtrate was charged to a clean reactor
7. 7
   workup.DISTILLATIONWater was distilled off under vacuum at 60° C
8. 8
   workup.STIRRINGto stir for 15 min
9. 9
   ろ過The solids were filtered
10. 10
    洗浄washed with 1-butanol (20 mL×2)
11. 11
    その他The product was dried to a constant weight at ˜65° C. under vacuum

実験手順

Oxycodone base (40.07 g) containing 4869 ppm of 14-hydroxycodeinone and 13.7 ppm DHDHC, was suspended in 1-butanol (250 mL) and water (180 mL) in a jacketed reactor. At 15° C. and with the reaction under nitrogen, aqueous hydrochloric acid (37%) was added to achieve a pH of 2.86. At 25° C., zinc dust (1 g) was added and the resulting mixture was stirred for 3 hr (Note: pH increased to ˜5.86 upon zinc powder addition). Activated carbon (Norit KB-G, 4 g) was added to the reactor and the solution was allowed to stir for 40 min. The reaction mixture was then filtered to remove the zinc and carbon. The filtrate was charged to a clean reactor. The pH of the solution was adjusted to 6.17 using pyridine (15 mL). Water was distilled off under vacuum at 60° C. The solution was then cooled to 20° C. and allowed to stir for 15 min. The solids were filtered and washed with 1-butanol (20 mL×2). The product was dried to a constant weight at ˜65° C. under vacuum to yield 42.14 g of crude oxycodone hydrochloride.

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