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Sodium Formate → N-[3-(4-Chlorophenyl)-8-hydroxy-2-isopropyl-4-oxo-4H-chromen-7-yl]formamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Formate | HCID 2723810 | — |
| 反応物 | 7-Amino-3-(4-chlorophenyl)-8-hydroxy-2-isopropyl-chromen-4-one | HCID 68701386 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 生成物 | N-[3-(4-Chlorophenyl)-8-hydroxy-2-isopropyl-4-oxo-4H-chromen-7-yl]formamide | HCID 59724241 | — |
反応手順
A stirred mixture of 7-amino-3-(4-chlorophenyl)-8-hydroxy-2-isopropyl-chromen-4-one (1.1 g, 3.35 mmol) and sodium formate (0.23 g, 3.35 mmol) in formic acid (50 ml) is heated under reflux for 2 h. After cooling to room temperature, the reaction mixture is poured into ice/water (300 ml) with stirring. The resulting aqueous suspension is washed with ethyl acetate (2×100 ml). The combined organic layers are washed with water (3×100 ml) and brine (100 ml), dried (magnesium sulfate) and filtered. The solvent is removed by evaporation in vacuo to afford a dark brown oil. This is purified by flash chromatography (hexane/ethyl acetate=1:1, followed by 100% ethyl acetate) to afford the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732435B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-808de5774aaf47ca9c8db9011397b39c |
| 出典メモ | uspto-grants-2010_06 |