化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 2-Amino-4-chloro-5-methylphenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Chloro-5-methyl-2-nitrophenol | HCID 23532 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Amino-4-chloro-5-methylphenol | HCID 104524 | 33.3% |
反応手順
To a solution of 4-chloro-5-methyl-2-nitrophenol (5.0 g) in methanol (100 mL) at 0° C. was added zinc powder (8.71 g), which was activated by hydrochloric acid in advance, and a solution of ammonium chloride (7.1 g) in water (20 mL). The suspension was stirred for 4 h at room temperature. Then the insoluble material was filtered off through celite, and the celite cake was washed with ethyl acetate (100 mL). The filtrate and washings were combined and concentrated under reduced pressure. The residue was purified by column chromatography over silica gel using hexane/ethyl acetate (3:2) to yield the title compound (1.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08889727B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-97d8b1235d82491fa0de0d796401146c |
| 出典メモ | uspto-grants-2014_11 |