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Piperidine → 3-Nitro-4-piperidin-1-ylpyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 4-Chloro-3-nitropyridine | HCID 2735781 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Nitro-4-piperidin-1-ylpyridine | HCID 3507669 | 95% |
反応手順
A solution of 4-chloro-3-nitropyridine (1.0 equiv.) and piperidine (2.0 equiv.) in ethanol, at a concentration of 0.5 M, was stirred at rt for 48 hours at which time the ethanol was removed in vacuo. The residue was partitioned between EtOAc (300 mL) and Na2CO3(sat) (75 mL), was washed further with H2O (50 mL), NaCl(sat.) (50 mL), was dried over MgSO4, was filtered and the volatiles were removed in vacuo yielding 3-nitro-4-(piperidin-1-yl)pyridine (95%). LCMS (m/z): 207.7 (MH+); LC Rt=1.60 min. 1H NMR (CDCl3): δ 8.80 (s, 1H), 8.31 (d, J=5.7, 1H), 6.84 (d, J=6.3, 1H), 3.18-3.21 (m, 4H), 1.64-1.78 (m, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822497B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-abee4ba2c18f413e9380fa98234b3b93 |
| 出典メモ | uspto-grants-2014_09 |