Hydrochloric Acid → Oxycodone Hydrochloride

HRID 84140

반응식

HRID 84140 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>O.C(O)(=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

6

반응물 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 5284603Oxycodone

생성물 1

HCID 5462350Oxycodone Hydrochloride수율 93%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

The first portion of purified Oxycodone base lot P (13.56 g, 43.0 mmol) was dissolved (in 80-mL beaker over 15 minutes) in a mixture of water (13 mL) and acetic acid (3 mL). 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, 93% yield on OC base purified) lot Q.

후처리

  1. stirringStirring
  2. waitwas continued for another 30 minutes
  3. filtrationPrecipitated product was filtered off
  4. washwashed
  5. filtrationon filter with IPA (2×20 ml) and acetone (2×20 mL)
  6. customdried
  7. filtrationon filter

출처 및 근거

ORD 기록
ord-c9088e28dfee4bb9a1438e5d7e3db7c5
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846923B1

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