関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | 1-(6,7-dihydro-4H-furo[3,2-c]pyridin-5-yl)-6-phenylhexan-1-one | HCID 19600041 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-(2-dimethylaminomethyl-6,7-dihydro-4H-furo[3,2-c]pyridin-5-yl)-6-phenylhexan-1-one | HCID 19600061 | — |
反応手順
To a solution of 0.403 g (1.355 mmol) of 1-(6,7-dihydro-4H-furo[3,2-c]pyridin-5-yl)-6-phenylhexan-1-one in 20 ml of acetic acid, 0.15 g (1.6 mmol) of 50% aqueous dimethylamine and 0.13 g (1.6 mmol) of 37% aqueous formaldehyde were added, followed by stirring at 100° C. for 15 minutes. After the solvent was distilled off under reduced pressure, the residual solution was alkalified with 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 column chromatography (ethyl acetate to ethyl acetate/methanol=4/1) 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-9f1f3d3a6f2a458daae6c6bbb59d3e2b |
|---|
| 出典メモ | uspto-grants-1999_12 |
|---|