化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 1-(6,7-dihydro-4H-furo[3,2-c]pyridin-5-yl)-6-phenylhexan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Diethyl cyanophosphonate | HCID 76257 | — |
| 反応物 | 6-Phenylhexanoic Acid | HCID 79695 | — |
| 反応物 | 4,5,6,7-Tetrahydrofuro[3,2-c]pyridine hydrochloride | HCID 19599941 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(6,7-dihydro-4H-furo[3,2-c]pyridin-5-yl)-6-phenylhexan-1-one | HCID 19600041 | — |
反応手順
To a solution of 0.250 g (1.566 mmol) of 4,5,6,7-tetrahydrofuro[3,2-c]pyridine hydrochloride, 0.33 g (1.7 mmol) of 6-phenylhexanoic acid and 0.87 ml (6.3 mmol) of triethylamine in 30 ml of dichloromethane, 0.36 ml (2.4 mmol) of diethyl cyanophosphonate was added dropwise under ice-cooling, followed by overnight stirring at room temperature. The reaction mixture was poured into aqueous sodium hydroxide and extracted with dichloromethane 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel chromatography (hexane/ethyl acetate=6/1 to 3/1) to yield the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05998433 |
| 出典データセット | uspto-grants-1999_12 |
| ORD ID | ord-6ec201416ced41c4bad2f6ecf37c45df |
| 出典メモ | uspto-grants-1999_12 |