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Trifluoroacetic anhydride → 4-chloro-2-fluoro-5-methyl-6-nitro-N-phenoxycarbonylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic anhydride | HCID 9845 | — |
| 反応物 | Ammonium nitrate | HCID 22985 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-chloro-2-fluoro-5-methyl-N-phenoxycarbonylaniline | HCID 18615647 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 4-chloro-2-fluoro-5-methyl-6-nitro-N-phenoxycarbonylaniline | HCID 18615646 | 103.1% |
反応手順
4-Chloro-2-fluoro-5-methyl-N-phenoxycarbonylaniline (7.1 g, 25.4 mmol) was dissolved in chloroform (68 ml) and trifluoroaceticanhydride (13.5 ml) and ammonium nitrate (2.4 g, 30.5 mmol) were slowly added with stirring at ambient temperature. The stirring was continued for 18 hr when a second batch of ammonium nitrate (0.4 g, 5 mmol) was added and stirring continued for 8 hr. Water was added and solution was neutralized by slow addition of sodium bicarbonate solution followed by extraction with chloroform. Organic layer was dried and evaporated under reduced pressure to afford an oily product (8.5 g) which was used for the next step without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06545161B2 |
| 出典データセット | uspto-grants-2003_04 |
| ORD ID | ord-4741a347fe21462983bdea91d7fc2dad |
| 出典メモ | uspto-grants-2003_04 |