関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 5-Bromo-1,3-difluoro-2-nitrobenzene | HCID 21335487 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Bromo-3-fluoro-N-methyl-2-nitroaniline | HCID 71652038 | — |
反応手順
2 M MeNH2 in THF (82 mL) was added dropwise to a solution of 5-bromo-1,3-difluoro-2-nitrobenzene (164 mmol) and Cs2CO3 (197 mmol) in THF (1 L). The reaction mixture was stirred at 0° C. for 1 h and then at room temperature for 1 h. The solvent was removed under reduced pressure. The residue was partitioned between EtOAc and H2O. The two phases were separated and the organic layer was dried (Na2SO4) and concentrated to afford the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09440929B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-dbfc8f0c4dbe4079969af08fe4403998 |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|