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Hexane → Methyl 5-bromo-2-(2-fluorophenylamino)-3,4-difluorobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Trimethylsilyldiazomethane | HCID 167693 | — |
| 反応物 | 5-Bromo-3,4-difluoro-2-((2-fluorophenyl)amino)benzoic acid | HCID 59519388 | — |
| 溶媒 | MeOH tetrahydrofuran | HCID 21899815 | — |
| 生成物 | Methyl 5-bromo-2-(2-fluorophenylamino)-3,4-difluorobenzoate | HCID 59519391 | 96% |
反応手順
To a solution of 5-bromo-2-(2-fluorophenylamino)-3,4-difluorobenzoic acid (30.3 mmol, 11 g) in THF:MeOH (60:20), cooled to 0° C., was added dropwise a solution of 2M TMSCHN2 in hexane (39.39 mmol, 19.7 ml). After the addition is completed, the reaction mixture was warmed to room temperature and stirred for an additional 4 hours. The crude reaction was quenched with acetic acid and extracted with EtOAc. The organic layers are combined, washed with H2O, dry over MgSO4 and concentrated under reduced pressure. The crude material was dried under vacuum and yields to 11 g (96%) of the title product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08063049B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-3ade5f9496bb432a814e32d597a3339b |
| 出典メモ | uspto-grants-2011_11 |