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Ethanol → Ethyl 2-amino-3-bromo-5-methylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 2-Amino-3-bromo-5-methylbenzoic acid | HCID 2774400 | — |
| 生成物 | Ethyl 2-amino-3-bromo-5-methylbenzoate | HCID 54594338 | 64% |
反応手順
Ethanol (10 mL) was added to 2-amino-3-bromo-5-methylbenzoic acid (1.00 g, 4.4 mmol). While the mixture was stirred, thionyl chloride (1.03 g, 8.7 mmol) was added at room temperature, followed by stirring at 80° C. overnight. The reaction solution was concentrated, and then diluted with water under ice-cooling, followed by extraction with ethyl acetate. The organic layer was washed with aqueous sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane=0/10, 4/6) to obtain 715 mg of the title compound as a pale yellow solid (64%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536197B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-afb07232ce8c4d14a2a461e01a8421a7 |
| 出典メモ | uspto-grants-2013_09 |