関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Methyl 5-bromo-2-methyl-3-nitrobenzoic acid | HCID 86623945 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl 3-bromo-5-nitrobenzoate | HCID 239341 | 104.6% |
反応手順
To stirred solution of 5-bromo-2,4-dimethyl-3-nitrobenzoic acid (13 g, 47.44 mmol) in DMF (120 mL), sodium carbonate (15 g, 142.2 mmol) and methyl iodide (4.4 ml, 71.16 mmol) were added. Resulting reaction mass was heated at 60° C. for 8 h. On completion, water was added to the reaction mass and extraction was carried out using ethyl acetate. Combined organic layers were washed with sat. bicarbonate solution and 5 N HCl, dried over sodium sulphate, concentrated under reduced pressure giving desired compound (12.9 g, 86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09376422B2 |
|---|
| 出典データセット | uspto-grants-2016_06 |
|---|
| ORD ID | ord-bf978c14db984630b8147a13eb9148b8 |
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| 出典メモ | uspto-grants-2016_06 |
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