化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Methyl 5-bromo-2-chloro-3-methoxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methyl 2-amino-5-bromo-3-methoxybenzoate | HCID 13894022 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 5-bromo-2-chloro-3-methoxybenzoate | HCID 58801718 | — |
反応手順
To a solution of compound 54 (27.0 g, 103 mmol) in H2O (70 mL) and conc.HCl (70 mL) was added dropwise a solution of NaNO2 (21.5 g, 311 mmol) in H2O (50 mL) at 0° C. After being stirred for 1 hour, a solution of Cu(I)Cl in conc.HCl (80 mL) was added to the reaction mixture dropwise at 0° C. The mixture was stirred at room temperature for 18 hours. To the mixture was added water (300 mL) and extracted with EtOAc (500 mL). The organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The crude product 55 was dried under high vacuum and used without further purification (29.0 g, 100%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09034921B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-619e1517e6714435a26d3efafd93cea2 |
| 出典メモ | uspto-grants-2015_05 |