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Sodium Hydroxide → 1-(2-Amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Aluminum;lithium;tetrachloride | HCID 166981 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | HCID 10611289 | HCID 10611289 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(2-Amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine | HCID 10587641 | 95.3% |
反応手順
A suspension of lithium aluminium chloride (8.2 g) in dry ether (170 ml) was treated dropwise with a solution of aluminium chloride (8.2 g) in ether (170 ml) under cooling. After stirring for half an hour at room temperature a solution of 1-(1,4-benzodioxan-5-yl)-4-cyanomethylpiperazine (9.4 g) in dry tetrahydrofuran (250 ml) was added dropwise at 15° C. After reflux for 1.5 h the mixture was cooled and conc. sodium hydroxide solution (40 ml) was added dropwise. Filtration and removal of solvent in vacuo gave an oil which was dissolved in methylene chloride and dried over magnesium sulfate. Removal of solvent in vacuo gave 1-(2-amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine (9.1 g) as a viscous oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05753661 |
| 出典データセット | uspto-grants-1998_05 |
| ORD ID | ord-f57bbf6bbd734e9ea6ce8740571c0f2c |
| 出典メモ | uspto-grants-1998_05 |