反応 #171321

ord-7c7a23c713a14c0b90d32055d5ea850c

試薬

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過catalyst was filtered off

実験手順

Pd/C Catalyst was filtered off and ammonium hydroxide was used for the oxycodone base precipitation (˜60 mL) at temperature less than 15° C. Precipitated product was washed with water (2×75 mL) and dried on filter giving 28.07 g of oxycodone base. The oxycodone base was transferred into 250-mL RBF with Pd/C catalyst (0.59 g) and water (120 mL). Formic acid (4.36 mL) was added (pH 2.1) and stirring continued for 45 minutes at 50-60° C. The reaction mixture was cooled to ambient temperature, catalyst was filtered off, and oxycodone base was isolated with ammonium hydroxide addition to the filtrate at temperature lower than 20° C. Drying on filter provided 29.51 g of the oxycodone base (2nd crude, Lot O).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08846923B1uspto-grants-2014_09