関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Acetylpyridine | HCID 14282 | — |
| 反応物 | (Benzyloxycarbonylmethyl)triphenylphosphonium bromide | HCID 11214019 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Benzyl 3-(4-pyridyl)-2-butenoate | HCID 67118931 | 42.4% |
反応手順
N,N-Dimethylformamide (33 ml) was added to a mixture of 4-acetylpyridine (2.00 g, 16.5 mmol) and (benzyloxycarbonyl)methyltriphenylphosphonium bromide (8.94 g, 18.2 mmol), and the whole was stirred under ice-cooling. Potassium carbonate (9.12 g, 66.0 mmol) was added thereto, the external temperature was raised to 70° C., and the whole was stirred overnight. The reaction mixture was diluted with diethyl ether (100 ml), and the whole was washed with water (100 ml, twice) and saturated brine (50 ml) successively. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 1.77 g (42%: mixture of E form and Z form) of benzyl 3-(4-pyridyl)-2-butenoate as a pale yellow oily matter.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07098226B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-0be49fb58b2f4f039baba09b76a48389 |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|