関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Methyl 2-amino-3-methoxybenzoate | HCID 602320 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 2-amino-5-bromo-3-methoxybenzoate | HCID 13894022 | 86% |
反応手順
To a solution of compound 53 (22.4 g, 123 mmol) in DMF (250 mL) was added N-bromosuccinimide (21.9 g, 123 mmol) portionwise at 0° C. The mixture was stirred at 0° C. for 0.5 h. To the mixture was added water and extracted with EtOAc (500 mL×2). The combined organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by silica gel column chromatography to provide the desired compound 54 (27.5 g, 86%) 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-dd0c574c13a842c8a23be71b3f6275b0 |
|---|
| 出典メモ | uspto-grants-2015_05 |
|---|
