Hydrochloric Acid → Oxycodone Hydrochloride

HRID 84142

반응식

HRID 84142 반응식
[CH3:1][N:2]1[C@@H:19]2[CH2:20][C:7]3[CH:8]=[CH:9][C:10]([O:22][CH3:23])=[C:11]4[O:12][C@H:13]5[C:14]([CH2:16][CH2:17][C@:18]2([OH:21])[C@:5]5([C:6]=34)[CH2:4][CH2:3]1)=[O:15].[ClH:24]>CC(O)C>[CH3:1][N:2]1[C@@H:19]2[CH2:20][C:7]3[CH:8]=[CH:9][C:10]([O:22][CH3:23])=[C:11]4[O:12][C@H:13]5[C:14]([CH2:16][CH2:17][C@:18]2([OH:21])[C@:5]5([C:6]=34)[CH2:4][CH2:3]1)=[O:15].[ClH:24]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 5284603Oxycodone

생성물 1

HCID 5462350Oxycodone Hydrochloride수율 93%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

As described above, oxycodone base purified (Lot P, 13.56 g, 43.0 mmol) was dissolved (in 80-mL beaker over 15 minutes) in the mixture of water (13 mL) and acetic acid (3.0 mL) at ambient temperature. Hydrochloric acid (10.41 mol/kg, 5.0 g or 51.6 mmol) was added to the solution over 5 minutes. Stirring was continued for another 40 minutes and IPA (55 mL) was added over 15 minutes. Stirring was continued for another 30 minutes. Precipitated product was filtered off, washed on filter with IPA (2×20 ml) and acetone (2×20 mL), dried on filter providing 14.74 g oxycodone HCl (39.86 mmol or 93% yield on OC base purified)—lot Q.

후처리

  1. custompurified (Lot P, 13.56 g, 43.0 mmol)
  2. dissolutionwas dissolved (in 80-mL beaker over 15 minutes)
  3. additionin the mixture of water (13 mL) and acetic acid (3.0 mL) at ambient temperature
  4. stirringStirring
  5. waitwas continued for another 30 minutes
  6. filtrationPrecipitated product was filtered off
  7. washwashed
  8. filtrationon filter with IPA (2×20 ml) and acetone (2×20 mL)
  9. customdried
  10. filtrationon filter

출처 및 근거

ORD 기록
ord-04ffbb1bc780463bbf4b1acebf235697
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846923B1

연결된 노트

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