Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Hydroxide → Oxycodone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | (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 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | Oxycodone | HCID 5284603 | 74.1% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846923B1 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-0924ff5c6bfd4539af6b02492c10d760 |
| 출처 메모 | uspto-grants-2014_09 |