化工社化工社 化学情報印刷レポート · 研究参考用
Nitric Acid → 5-Chloro-2-methyl-3-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 5-Chloro-2-methylbenzoic acid | HCID 82009 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 5-Chloro-2-methyl-3-nitrobenzoic acid | HCID 23009762 | 78.9% |
反応手順
To a conc. H2SO4 (90 mL) was added portionwise 5-chloro-2-methylbenzoic acid (13.2 g, 77.6 mmol) at −5˜0° C. Then a mixture of conc. HNO3 (10.5 g, 1744 mmol) in conc. H2SO4 (15 mL) was added dropwise at −5˜0° C. over a period of about 1.5 hr. After the addition, the mixture was stirred at this temperature for 2 hr. The mixture was poured into crashed ice with vigorous stirring and the precipitate was collected by filtration. The precipitate was dissolved in EtOAc, washed with brine, dried over anhydrous Na2SO4, and concentrated to give a crude title compound (13.2 g), which was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08999987B2 |
| 出典データセット | uspto-grants-2015_04 |
| ORD ID | ord-520faaba99414ee986fd8ebec9890b2d |
| 出典メモ | uspto-grants-2015_04 |