関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | 1-(5,7-dihydro-4H-furo[2,3-c]pyridin-6-yl)-6-phenylhexan-1-one | HCID 19600145 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-(2-diethylaminomethyl-5,7-dihydro-4H-furo[2,3-c]pyridin-6-yl)-6-phenylhexan-1-one | HCID 19600122 | — |
反応手順
To a solution of 0.322 g (1.083 mmol) of 1-(5,7-dihydro-4H-furo[2,3-c]pyridin-6-yl)-6-phenylhexan-1-one in 20 ml of acetic acid, 0.13 g (1.3 mmol) of diethylamine and 0.11 g (1.3 mmol) of 37% aqueous formaldehyde were added, followed by stirring at 100° C. for 1.5 hours. 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 |
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| 特許番号 | US05998433 |
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| 出典データセット | uspto-grants-1999_12 |
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| ORD ID | ord-14f5b9ca8a61463a959f249b7019aef9 |
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| 出典メモ | uspto-grants-1999_12 |
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