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Methanol → 5-(Methoxycarbonyl)-2-methylbenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4-Methylbenzene-1,3-dicarboxylic acid | HCID 595750 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 5-(Methoxycarbonyl)-2-methylbenzoic acid | HCID 22999486 | — |
反応手順
A mixture of compound (2) (2.83 g, 15.71 mmol), thionyl chloride (50 ml) and DMF (3 drops) was heated at reflux for 2 hours. After cooling to room temperature, excess thionyl chloride was removed under reduced pressure (rotary evaporator). The dark oil which was obtained was dissolved in carbon tetrachloride (30 ml), treated with pyridine (1 ml, 12.43 mmol) and methanol (20 ml) and stirred at ambient temperature for 2 hours. The solvents were evaporated and the residue purified by flash chromatography: silica, hexane/EtOAc (9:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06610269B1 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-3c7986863cd943adb62352da01f11da9 |
| 出典メモ | uspto-grants-2003_08 |