化工社化工社 化学情報印刷レポート · 研究参考用
Ammonium Hydroxide → Oxycodone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | (4R,4aS,7aR,12bS)-4a-hydroxy-9-methoxy-3-methyl-2,4,5,6,7a,13-hexahydro-1H-4,12-methanobenzofuro[3,2-e]isoquinolin-7-one acetate | HCID 86762802 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Oxycodone | HCID 5284603 | 74.1% |
反応手順
Oxycodone acetate solution was diluted with isopropanol (25 mL), cooled to ˜10° C. and neutralized at 10° C. to 5° C. with ammonium hydroxide (conc., ˜30 mL until pH ˜9.5). Stirring continued for 10 minutes and precipitated solids were filtered off, washed on filter with water (20 mL, 2×50 mL, 10 mL) and dried on filter for 0.5 hours. The light gray wet material (22.29 g) was prepared. This material was dissolved in chloroform (150 mL), treated with sodium sulfate (anhydrous) for one hour. Solvent was removed in vacuum and gray powder was dried on rotary evaporator for one hour at 50° C. in the bath, providing oxycodone base (16.31 g, 51.72 mmol, 74.1% yield on ABUK sulfate). Impurity profile is shown in Table 8.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09108976B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-22325de47b0246688eddb04eeb273aa9 |
| 出典メモ | uspto-grants-2015_08 |