化工社化工社 化学情報印刷レポート · 研究参考用
Water → Ammonium Hydroxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Oxycodone | HCID 5284603 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 生成物 | Ammonium Hydroxide | HCID 14923 | — |
| 生成物 | Oxycodone | HCID 5284603 | — |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846923B1 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-7c7a23c713a14c0b90d32055d5ea850c |
| 出典メモ | uspto-grants-2014_09 |