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Methyl iodide → Methyl 2-methyl-6-nitrobenzoate
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 | 6-Methyl-2-nitrobenzoic acid | HCID 16097 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | Methyl 2-methyl-6-nitrobenzoate | HCID 596057 | — |
反応手順
To a solution of the 2-methyl-6-nitro-benzoic acid (5.6 g, 30.9 mmol, 1.0 eq, Aldrich) and acetone (100 mL) was added crushed K2CO3 (21.4 g, 154.6 mmol, 5 eq) and MeI (9.6 mL, 154.6 mmol, 5.0 eq.). The reaction was heated to reflux for 15 h then cooled to RT, filtered and concentrated in vacuo. The filtrate was dissolved in EtOAc, washed with H2O and brine, dried (MgSO4) and concentrated in vacuo to give the desired compound as a reddish-brown oil which upon standing at RT crystallized as tan needles.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07390820B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-ca3edb7fbf8848eeaa728149acea2bb2 |
| 出典メモ | uspto-grants-2008_06 |