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4-Chloropyridine hydrochloride → 4-Acetylamino-1-(4-pyridyl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloropyridine hydrochloride | HCID 81852 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-Acetamidopiperidine dihydrochloride | HCID 11401105 | — |
| 溶媒 | Isoamyl Alcohol | HCID 31260 | — |
| 生成物 | 4-Acetylamino-1-(4-pyridyl)piperidine | HCID 18918435 | — |
反応手順
A mixture of the product from step (ii) (1.79 g), 4-chloropyridine hydrochloride (1.50 g), sodium hydrogen carbonate (2.86 g) in 3-methyl 1-butanol (25 ml) was heated at reflux temperature for 16 hours. The cooled mixture was filtered and the filtrate concentrated in vacuo. Purification of the residue by flash chromatography on silica, eluting with methanol/dichloromethane (1:2 v/v) gave 4-acetylamino-1-(4-pyridyl)piperidine as a foam, 0.69 g: NMR(d6DMSO) δ 8.10(2H,d), 7.80(1H,bd), 6.80(2H,dd), 3.82(3H,m), 2.93(2H,dt), 1.78(3H,s), 1.77(2H,m), 1.33(2H,dq); m/e 220 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728701 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-a48b81fc6740494aa3b8c87fee1bf7d7 |
| 出典メモ | uspto-grants-1998_03 |