化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → 2-Amino-4-chloro-5-(trifluoromethyl)phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4-Chloro-2-nitro-5-(trifluoromethyl)phenol | HCID 66879688 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Amino-4-chloro-5-(trifluoromethyl)phenol | HCID 66880478 | 84.4% |
反応手順
A mixture of 2.3 g of 4-chloro-2-nitro 5-trifluoromethylphenol and 10 ml of ethyl acetate was added dropwise to a mixture, which was heated to 80° C., of 2.6 g of electrolytic iron, 10 ml of acetic acid and 20 ml of water, and then the reaction mixture was stirred for one hour. The mixture was cooled to room temperature, and then water was added, followed by extraction with ethyl acetate. The combined organic layers were washed with water, a saturated aqueous solution of sodium hydrogencarbonate and a saturated sodium chloride solution, dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 1.7 g of 2-amino-4-chloro-5-trifluoromethylphenol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08445522B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-8424177f45f747529a84be62afd6b4e7 |
| 出典メモ | uspto-grants-2013_05 |