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Potassium Iodide → 1-(1,4-Benzodioxan-5-yl)-4-(2-(2,2-dimethoxy-1-ethylamino)-1-ethyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Acetaldehyde, bromo- | HCID 105131 | — |
| 反応物 | 1-(2-Amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine | HCID 10587641 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethylacetate methanol | HCID 21584119 | — |
| 生成物 | 1-(1,4-Benzodioxan-5-yl)-4-(2-(2,2-dimethoxy-1-ethylamino)-1-ethyl)piperazine | HCID 70290042 | — |
反応手順
A mixture of 1-(2-amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine (9.1 g), bromoacetaldehyde dimethylacetale (6.5 g), potassium iodide (0.5 g), and potassium carbonate (4.8 g) in 1,4-dioxan (200 ml) was refluxed for 16 h. Water was added followed by extraction with ethyl acetate. The organic phase was concentrated in vacuo leaving an oil which was applied to a silica gel column (eluent: ethyl acetate/methanol=1:3). The product, 1-(1,4-benzodioxan-5-yl)-4-[2-(2,2-dimethoxy-1-ethylamino)-1-ethyl]piperazine, was obtained as an oil (4.7 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06140331 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-a9408372408f465faf1f6e2346ffb2fa |
| 出典メモ | uspto-grants-2000_10 |