反応 #602761

ord-828f19dd148b4f9883eb4558afe2355c

反応方程式

COc1ccc2c3c1O[C@H]1C(=O)CC[C@@]4(O)[C@@H](C2)N(C)CC[C@]314
oxycodone
O
water
COc1ccc2c3c1O[C@H]1C(=O)CC[C@@]4(O)[C@@H](C2)N(C)CC[C@]314
oxycodone
[NH4+].[OH-]
ammonium hydroxide

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: US09108976B2uspto-grants-2015_08