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Dimethylformamide → Methyl 2-methoxy-5-methylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 5-Methylsalicylic acid | HCID 6973 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 生成物 | Methyl 2-methoxy-5-methylbenzoate | HCID 10241396 | 95% |
反応手順
To 5-methylsalicylic acid (3.04 g, 20 mmol) in DMF (100 ml) were added potassium carbonate (8.28 g, 60 mmol) and iodomethane (6.24 g, 44 mmol) under ice cooling and then the mixture was stirred at room temperature for 12 hours. The mixture were extracted by adding 5% sodium hydrogensulfite and ethyl acetate, and the extracted organic layer was washed with 5% citric acid and 5% brine. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography (hexane-ethyl acetate) to give the captioned compound (3.43 g, 19.1 mmol, yield: 95%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08148371B2 |
| 出典データセット | uspto-grants-2012_04 |
| ORD ID | ord-613ae75cdef8470297752cd83c854a83 |
| 出典メモ | uspto-grants-2012_04 |