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Benzylethanolamine → Tert-butyl 2-(benzyl (2-hydroxyethyl)amino)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzylethanolamine | HCID 4348 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | tert-Butyl bromoacetate | HCID 79177 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Tert-butyl 2-(benzyl (2-hydroxyethyl)amino)acetate | HCID 15817339 | — |
反応手順
tert-Butyl bromoacetate (32.3 ml; 0.2 mol) is slowly added dropwise, while cooling in ice, to a solution of N-benzylethanolamine (30.2 g; 0.2 mol) and triethylamine (27.9 ml; 0.2 mol) in anhydrous N,N-dimethylformamide (200 ml). The mixture is stirred at room temperature for 22 h and is then concentrated in vacuo. The residue is subsequently distilled repeatedly with toluene. The resulting oil is taken up in dichloromethane (400 ml) and extracted twice by shaking with water (160 ml on each occasion). The organic phase is dried (magnesium sulphate) and concentrated. Yield: 47.8 g (90%), colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05623049 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-21aed8d69531446db839dc358717fabb |
| 出典メモ | uspto-grants-1997_04 |