関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | 4-Fluoro-3-nitrobenzoic acid | HCID 67987 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | Ethyl 4-fluoro-3-nitrobenzoate | HCID 21277355 | — |
反応手順
A solution of 4-fluoro-3-nitrobenzoic acid (Alfa Aesar, 10.0 g, 54 mmol) and concentrated H2SO4 (0.2 ml, 4.1 mmol) in EtOH (200 ml) was refluxed for 40 h. The mixture was cooled to 0° C., solid NaHCO3 and MgSO4 was added, and the suspension was filtered and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→30% EtOAc-hexanes) to yield the title compound as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524917B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-c474b033b567489bbfa0e0a712e1b26f |
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| 出典メモ | uspto-grants-2013_09 |
|---|