化工社化工社 化学情報印刷レポート · 研究参考用
3,5-Dichloroaniline → 3,5-Dichloro-2-iodoaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,5-Dichloroaniline | HCID 12281 | — |
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Acetic acid methylene chloride | HCID 21922555 | — |
| 生成物 | 3,5-Dichloro-2-iodoaniline | HCID 10016943 | 45.7% |
反応手順
Dissolve 3,5-dichloroaniline (10 g, 61.5 mmol) in 1:1 acetic acid/methylene chloride (200 mL). Add N-iodosuccinimide (16.9 g, 61.5 mmol) as a solid and stir at room temperature in the absence of light for 8 hours. Pour the solution into saturated sodium hydrogen carbonate (200 mL) and extract into methylene chloride (100 mL). Wash with saturated sodium hydrogen carbonate (200 mL), dry (MgSO4) and evaporate the solvent in vacuo. Purify by silica gel chromatography to give the title compound (8.1 g, 45%); mp 61°-63° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05484814 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-5a73e3d4f0ea4a83ac240edfe093d315 |
| 出典メモ | uspto-grants-1996_01 |