반응 #2360066

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Oxymorphone

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Oxymorphone

6α-oxymorphol

6β-oxymorphol

용매

1-propanol

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후처리

1. 1
   workup.ADDITIONwas charged
2. 2
   기타was lowered to 25±5° C.
3. 3
   workup.STIRRINGstirred for 1 h
4. 4
   온도The batch was further cooled to 10±5° C.
5. 5
   workup.STIRRINGstirred 1 h
6. 6
   여과The product was collected by filtration
7. 7
   세척washing the cake with 1-propanol (10±5° C., 2×48.2 g)
8. 8
   기타then drying under vacuum at 55±5° C.

실험 절차

The crude Oxymorphone Base (267.7 g wet, 180.1 g dry basis) was transferred back to a clean 3000 mL reaction vessel and 1-propanol (321.6 g) was charged. The slurry was heated to 90±3° C. and stirred for 1.5 h. The temperature was lowered to 25±5° C. and stirred for 1 h. The batch was further cooled to 10±5° C. and stirred 1 h. The product was collected by filtration washing the cake with 1-propanol (10±5° C., 2×48.2 g) then drying under vacuum at 55±5° C. to give Oxymorphone Base (167.8 g, 83.3% yield, 99.9 area %, 6α-oxymorphol 0.11 area %, 6β-oxymorphol not detected).

출처