関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Bromophenol | HCID 7808 | — |
| 反応物 | furo(3,4-b)pyridin-5(7H)-one | HCID 819439 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-[(4-Bromophenoxy)methyl]nicotinic acid | HCID 57754429 | — |
反応手順
32 g (185 mmol) of 4-bromophenol are treated in methanol with 33.32 g (185 mmol) of 30% solution of sodium methoxide in methanol. The solvent is eliminated and the residue mixed with 5.0 g (37.00 mmol) of furo[3,4-b]pyridin-5(7H)-one (prepared according to Synthesis, 1997, 113-116). The system is stirred at 165° C. for 30′ (at first the mixture melts, afterwards solidifies). Once at room temperature, the solid is dissolved in excess water, adjusted at pH 7-8 with 2N HCl and extracted two times with dichloromethane. The aqueous layer is adjusted at pH 5-6 with more 2N HCl and the solid that precipitates is filtered, washed with water and dried. The yield is 6.6 g (58%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07557212B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-2ac9279014114907a916be1f6da53216 |
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| 出典メモ | uspto-grants-2009_07 |
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