関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 反応物 | 2-Acetylpyridine | HCID 14286 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(1-Dimethylamino ethyl)pyridine | HCID 14810987 | — |
反応手順
A suspension of g 1.21 (0.01 moles) of 2-acetylpyridine, 1.63 (0.02 moles) of dimethylamine hydrochloride, g 0.63 (0.01 moles) of NaCNBH3 and g 0.4 (0.01 moles) of NaOH in ml.80 of dry methanol was stirred at room temperature for 4 days. The insoluble matter was filtered off and the filtrate was made strongly alkaline with 15% aqueous NaOH. After evaporation of the mathanol, some NaOH pellets were added into the aqueous residue, and the solution was extracted with ether. The combined ethereal solutions were dried on solid NaOH and evaporated i.v. The oily residue (gr 2.8) was chromatographed on 12 g. of silicagel, eluting with CH2Cl2 containing 2% to 10% methanol. 1.7 g. of oily product were obtained, sufficiently pure for the subsequent step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04879300 |
|---|
| 出典データセット | uspto-grants-1989_11 |
|---|
| ORD ID | ord-8c51d20fbb7948968cb6868f2d6fba9a |
|---|
| 出典メモ | uspto-grants-1989_11 |
|---|