関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Iodine chloride | HCID 24640 | — |
| 反応物 | 2-Chloro-4-trifluoromethylaniline | HCID 162001 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Chloro-6-iodo-4-(trifluoromethyl)aniline | HCID 56587696 | 97.1% |
反応手順
Iodine monochloride (17.2 g, 108 mmol) in hydrochloric acid (36%, 21.4 g) and water (35 mL) was added dropwise to 2-chloro-4-(trifluoromethyl)benzenamine (20.0 g, 102 mmol) in hydrochloric acid (36%, 20.7 g) and water (140 mL). The mixture was warmed to 50° C. for a total of 8 h. Sodium hydroxide (50%, 33.5 g, 419 mmol) was added to the mixture at room temperature. The mixture was extracted with dichloromethane (2×250 mL), and the extracts were dried and evaporated to give the product as an oil (31.83 g, 97% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09035101B2 |
|---|
| 出典データセット | uspto-grants-2015_05 |
|---|
| ORD ID | ord-9db113ea38b14b2ea96e8bc669de7892 |
|---|
| 出典メモ | uspto-grants-2015_05 |
|---|
