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Water → Ethyl 2-(4-(3-nitrophenyl)-1-piperazinyl)-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-(3-Nitrophenyl)piperazine | HCID 2760216 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 2-(4-(3-nitrophenyl)-1-piperazinyl)-acetate | HCID 22330178 | 65% |
反応手順
To a solution of 1-(3-nitrophenyl)piperazine (12.0 g; 58 mmol) in DMF (60 ml) was added sodium hydride (2.55 g; 64 mmol, 60% dispersion in mineral oil) in portions over 30 min. The mixture was kept under nitrogen. Ethyl 2-bromoacetate (7.1 ml; 64 mmol) was added, the mixture was stirred at ambient temperature for one hour and then poured into water (250 ml). The oily precipitate was filtered off, re-dissolved in ethyl acetate and washed with water. The organic phase was dried over magnesium sulphate and evaporated to dryness to leave 6b (11.0 g; 65%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06936613B2 |
| 出典データセット | uspto-grants-2005_08 |
| ORD ID | ord-6d14ea4e45ad4f558db074e4354f61ef |
| 出典メモ | uspto-grants-2005_08 |