関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Aminopyridine | HCID 10439 | — |
| 反応物 | 4-Fluorobenzyl bromide | HCID 68021 | — |
| 反応物 | Ethyl 2-bromo-3-phenylpropanoate | HCID 4737529 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 18008032 | HCID 18008032 | 1% |
反応手順
630 mg (6.7 mmol) of 2-aminopyridine and 1.72 g (6.7 mmol) of ethyl 2-bromo-3-phenylpropionate were refluxed under heating in 50 ml of ether for 12 hours. The reaction mixture was allowed to cool to room temperature and ether was removed by decantation. The residue was added with and dissolved in 30 ml of absolute ethanol, which was added to a solution of 150 mg (6.5 mmol) of sodium in 10 ml of absolute ethanol and stirred at room temperature for one hour. Then, 0.8 ml (6.5 mmol) of 4-fluorobenzylbromide was added and stirred for overnight. The reaction mixture was added to ice water and extracted with methylene chloride. Then, the solvent was removed under reduced pressure and the residue was purified with silica gel column chromatography, thus obtaining 22 mg (yield: 1%) of the titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06635652B1 |
|---|
| 出典データセット | uspto-grants-2003_10 |
|---|
| ORD ID | ord-341b7fbd82a845f494565c5adfd8bd14 |
|---|
| 出典メモ | uspto-grants-2003_10 |
|---|