関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| 反応物 | 2-Chloropyridine--hydrogen chloride (1/1) | HCID 15619920 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Boc-4-(2-pyridyloxy)piperidine | HCID 21906039 | 72% |
反応手順
1-t-Butoxycarbonyl-4-piperidinol (5.0 g 24.88 mmol) in dry dimethylformamide (60 ml) was treated with sodium hydride (60% 2.99 g 74.75 mmol) at room temperature under argon and then with 2-chloropyridine hydrochloride (4.1 g 27.33 mmol). Then mixture was heated at 80° C. overnight. After cooling the reaction was carefully quenched with water (5 ml) and then diluted with more water (20 ml) and extracted with ethyl acetate (30 ml). The organic solution was washed with sat. sodium bicarbonate, dried (MgSO4) and evaporated to give 1-t-butoxycarbonyl-4-(2-pyridoxy)piperidine (4.96 g 72%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06855715B1 |
|---|
| 出典データセット | uspto-grants-2005_02 |
|---|
| ORD ID | ord-390aae966993417181c270dae2276020 |
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| 出典メモ | uspto-grants-2005_02 |
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