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1,4-Diazabicyclo(3.2.2)nonan-3-one → 1,4-Diazabicyclo(3.2.2)nonane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,4-Diazabicyclo(3.2.2)nonan-3-one | HCID 4401850 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,4-Diazabicyclo(3.2.2)nonane | HCID 398407 | 64.5% |
反応手順
Lithium aluminum hydride (2.0 g, 51.4 mmoles) was slurried in 250 ml of dry tetrahydrofuran and 3-oxo-1,4-diazabicyclo[3.2.2]nonane (3.6 g, 25.7 mmoles) was added carefully as a solid in one portion at room temperature. The resulting mixture was then heated to a gentle reflux for 20 hours. The reaction was cooled to room tempeature and quenched by slow addition of 2.5 ml water. The salts were filtered and washed several times with diethyl ether totaling 1.0 1. These washings and the supernatant were combined, dried over magnesium sulfate and concentrated to give 2.09 g (64.5%) of the title compound as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04775668 |
| 出典データセット | uspto-grants-1988_10 |
| ORD ID | ord-c29499e62b974f038a1fcb19a31047d6 |
| 出典メモ | uspto-grants-1988_10 |