反応 #171322

反応方程式

Oxycodone

Hydrochloric acid

IPA

→

oxycodone HCl

収率 93.0%

溶媒

water

acetic acid

反応条件

後処理

1. 1
   workup.STIRRINGStirring
2. 2
   workup.WAITwas continued for another 30 minutes
3. 3
   ろ過Precipitated product was filtered off
4. 4
   洗浄washed
5. 5
   ろ過on filter with IPA (2×20 ml) and acetone (2×20 mL)
6. 6
   その他dried
7. 7
   ろ過on filter

実験手順

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.

出典