化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Carbonate → 2-Methyl-1-azabicyclo(2.2.2)octan-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Methylene-3-quinuclidinone hydrochloride hydrate | HCID 16219655 | — |
| 触媒 | Adams' catalyst | HCID 345198 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Methyl-1-azabicyclo(2.2.2)octan-3-one | HCID 12381698 | 58% |
反応手順
A mixture of 10.1 g (58.4 mmol) of 2-methylene-1-azabicyclo[2.2.2]octan-3-one hydrochloride hydrate, 8.1 g of K2CO3 and 100 mg of PtO2 in 100 mL of MeOH was hydrogenated at 10–15 psi H2 for about 1 hr. The solution was filtered through dicalite and the solvent was evaporated in vacuo. The residue was dissolved in CHCl3 and again filtered through dicalite. The filtrate was evaporated in vacuo to give 4.7 g (58% yield) of 2-methyl-1-azabicyclo[2.2.2]octan-3-one Compound 8A as a yellow oil. 1H NMR (CDCl3) 1.3 (d, 3H), 2.0 (m, 4H), 2.4 (t, 1H), 2.9 (m, 1H), 3.05 (, 1H), 3.2 (m, 3H). This material was used without further purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07179818B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-dcc4f9d586d94235b4790ce949c04575 |
| 出典メモ | uspto-grants-2007_02 |