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Methyl iodide → 2-Chloro-3-methoxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloro-3-hydroxybenzaldehyde | HCID 593376 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chloro-3-methoxybenzaldehyde | HCID 12575695 | — |
反応手順
To a solution of 2-chloro-3-hydroxybenzaldehyde (4.55 g, 29 mmol) in DMF (30 mL) was added K2CO3 (4.8 g, 34.9 mmol) followed by MeI (2.7 mL, 43.6 mmol), and the mixture was stirred at room temperature for 16 hours. Following concentration in vacuo, the residual was taken up in ethyl acetate, washed with H2O, brine, dried over Na2SO4, and concentrated. Purification by column chromatography on silica gel with ethyl acetate/hexanes 1/5 afforded 2-chloro-3-methoxybenzaldehyde 7a (4.68 g, 94%) as a colorless oil, which solidified upon standing. GCMS (EI) m/z 170, 172 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07419983B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-10805d73e11e460d8cdc089914c1dbde |
| 出典メモ | uspto-grants-2008_09 |