反応 #602764

反応方程式

oxycodone

Hydrochloric acid

→

oxycodone HCl

収率 93.0%

溶媒

IPA

反応条件

後処理

1. 1
   その他purified (Lot P, 13.56 g, 43.0 mmol)
2. 2
   workup.DISSOLUTIONwas dissolved (in 80-mL beaker over 15 minutes)
3. 3
   workup.ADDITIONin the mixture of water (13 mL) and acetic acid (3.0 mL) at ambient temperature
4. 4
   workup.STIRRINGStirring
5. 5
   workup.WAITwas continued for another 30 minutes
6. 6
   ろ過Precipitated product was filtered off
7. 7
   洗浄washed
8. 8
   ろ過on filter with IPA (2×20 ml) and acetone (2×20 mL)
9. 9
   その他dried
10. 10
    ろ過on filter

実験手順

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.

出典