関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 3,4-Dichlorophenol | HCID 7258 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4,5-Dichloro-2-nitrophenol | HCID 38248 | 46.1% |
反応手順
A 250 mL roundbottom flask charged with 3,4-dichlorophenol (3.053 g, 18.7 mmol) in 50 mL CH2Cl2 was cooled to 0° C. in an ice bath. To the stirred solution was added concentrated H2SO4 (1.56 mL, 28.1 mmol). The solution became turbid. To this mixture was added concentrated HNO3 (1.2 mL, 18.7 mmol), dropwise and carefully to maintain a temperature below 5° C. The reaction was stirred for 30 min at 0° C., then cooled with an ice bath and quenched with 150 mL H2O. The layers were separated and the aqueous layer was extracted once with 35 mL CH2Cl2. The combined organics were dried over anhydrous Na2SO4, concentrated under vacuum and purified using flash chromatography (10% EtOAc/hexanes as eluent) to yield the desired nitrophenol as a bright yellow solid (1.793 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08093244B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-680615b7477842b8aa48480eb61d4e21 |
|---|
| 出典メモ | uspto-grants-2012_01 |
|---|