化工社化工社化学信息打印报告 · 仅供科研参考
氨 → 内向-3-氨基-9-甲基-9-氮杂双环[3,3,1]壬烷
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 氨 | HCID 222 | — |
| 反应物 | 高托品酮肟 | HCID 3219133 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 产物 | 内向-3-氨基-9-甲基-9-氮杂双环[3,3,1]壬烷 | HCID 11008150 | 93% |
反应步骤
A solution of 9-methyl-9-azabicyclo[3.3.1]nonan-3-one oxime (10 g, 0.06 moles) in methanol (70 ml) and 0.88 ammonia; (36 ml; 10.0 equivs) was hydrogenated at 50° C. and 50 psi (344.8 kPa)/H2 for 16 hrs using 5% Rhodium on carbon paste (1 g dry weight). The reaction mixture was cooled to room temperature and filtered to remove catalyst. The catalyst bed was washed with methanol and the methanolic solution was then evaporated under reduced pressure to give the title compound as an oil (8.6 g, 93% weight recovery) which solidified to a waxy solid on standing (8.6 g, 93%).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05856489 |
| 来源数据集 | uspto-grants-1999_01 |
| ORD ID | ord-cc0d3a87311340899db2f5ecccf0561d |
| 来源说明 | uspto-grants-1999_01 |