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Methanol → Methyl 2-iodo-3-nitrobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-Iodo-3-nitrobenzoic acid | HCID 220966 | — |
| 生成物 | Methyl 2-iodo-3-nitrobenzoate | HCID 264093 | 95% |
反応手順
A mixture of 2-iodo-3-nitrobenzoic acid (31.0 g, 106 mmol) and concentrated sulfuric acid (24.9 mL, 317 mmol) in methanol (600 mL) was heated under reflux for 12 hr. The solvent was evaporated under reduced pressure and the residue was extracted with methylene chloride. The extract was washed with saturated aqueous sodium hydrogen carbonate solution and water, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by recrystallization (chloroform/hexane) to give the title compound (31.0 g, yield 95%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08110585B2 |
| 出典データセット | uspto-grants-2012_02 |
| ORD ID | ord-3bbcf3c1b3e24be1a290d59631cecc6a |
| 出典メモ | uspto-grants-2012_02 |