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Sulfuric Acid → 2-(Methoxycarbonyl)-6-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 3-Nitrophthalic acid | HCID 69043 | — |
| 反応物 | Methylorthoformate | HCID 53629101 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(Methoxycarbonyl)-6-nitrobenzoic acid | HCID 4399477 | 82.2% |
反応手順
To a suspension of 3-nitrophthalic acid (211 g) and methyl orthoformate (127 g) in methanol (420 ml) was added conc. sulfuric acid (20 ml) dropwise with stirring. The reaction mixture was heated under reflux for 18 hours and concentrated to dryness. After addition of water (30 ml) to the residue, the mixture was stirred at 3-10° C. for one hour. The precipitated crystals were recrystallized from ethyl acetate-hexane to give pale yellow prisms (185 g, 82%), m.p. 166-168° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06608210B2 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-2f0dbddde74b41fda6b195d8e1e9af4f |
| 出典メモ | uspto-grants-2003_08 |