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Sulfuric Acid → 2-(2-Nitro-4-trifluoromethylphenoxy)-4,5-dichlorobenzenesulfonic acid, ammonium salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-(2-Nitro-4-trifluoromethylphenoxy)-4,5-dichlorobenzene | HCID 1343009 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(2-Nitro-4-trifluoromethylphenoxy)-4,5-dichlorobenzenesulfonic acid, ammonium salt | HCID 15407327 | — |
反応手順
Fuming sulfuric acid (8 mililiter (hereinafter mL) was cooled to -20° C. and 2-(2-nitro-4-trifluoromethyl-phenoxy)-4,5-dichlorobenzene (8 g, 22.8 mmol) in methylene chloride (8 mL) was added to the solution. The mixture was stirred for 15 min and then quenched in ice. Extraction with ethyl acetate followed by flash chromatography (silica gel, methylene chloride/isopropanol/ammonium hydroxide) gave the title compound. 1H NMR (400 MHz, CD3OD) δ8.31 (d, 1H), 8.11 (s, 1H), 7.87 (dd, 1H), 7.4 (s, 1H), 7.16 (d, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05470882 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-6859ae352e57456b9de7da9afed7fde4 |
| 出典メモ | uspto-grants-1995_11 |