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Nitromethane → Ethyl 4-hydroxy-4-(nitromethyl)-1-piperidinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitromethane | HCID 6375 | — |
| 反応物 | Ethyl 4-oxo-1-piperidinecarboxylate | HCID 34767 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 4-hydroxy-4-(nitromethyl)-1-piperidinecarboxylate | HCID 22708806 | — |
反応手順
To a solution of N-carbethoxy-4-piperidone (11.34 g, 66.24 mmol) in nitromethane (5.3 mL) and ethanol (2 mL) was added a solution of sodium ethoxide in ethanol (2.67 M, 1.24 mL, 3.31 mmol). The mixture was stirred for 5 min and a solution formed from which a solid precipitated. After 1.5 h, water (100 mL) was added and the solid was isolated by filtration, washed with water (100 mL), and dried under vacuum with heat to yield the product ethyl 4-hydroxy-4-(nitromethyl)piperidine-1-carboxylate as an off white solid, 9.58 g (62%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541438B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-01e93de79b1c4700b1b095c0e4fd6300 |
| 出典メモ | uspto-grants-2013_09 |