化工社化工社 化学情報印刷レポート · 研究参考用
Methyl iodide → Methyl 3-methoxy-4-methyl-2-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 | 3-Hydroxy-4-methyl-2-nitrobenzoic acid | HCID 81374 | — |
| 反応物 | Dichloromethane methanol | HCID 21226129 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 3-methoxy-4-methyl-2-nitrobenzoate | HCID 14543060 | 94.7% |
反応手順
To a solution of 3-hydroxy-4-methyl-2-nitrobenzoic acid (365 g, 1.85 mol) in DMF (3280 mL) were added K2CO3 (524.4 g, 3.80 mol) and MeI (788 g, 5.55 mol) in one portion. Then the reaction mixture was stirred at room temperature overnight. TLC(CH2Cl2/MeOH=3:1) indicated the reaction was complete. Water (9 L) was added to the reaction mixture and the mixture was extracted with EtOAc (3 L×2). The combined organic layers were washed with 1 N aq. NaOH (1 L×2) and brine, dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound (395 g, 94.7%) as a light yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07998978B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-bc9a8d433be54c0487e702831b7e51a7 |
| 出典メモ | uspto-grants-2011_08 |