関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Fluoro-2-nitrobenzene | HCID 73895 | — |
| 反応物 | Tert-butyl 2-amino-2-methylpropanoate hydrochloride | HCID 12186776 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 59497651 | HCID 59497651 | 50% |
反応手順
To a mixture of 1-fluoro-2-nitrobenzene (485 μL, 4.6 mmol) and 2-amino-2-methyl-propionic acid tert-butyl ester hydrochloride (1.0 g, 5.1 mmol) in DMF (5 mL) was added Et3N (1.3 mL, 9.3 mmol). The mixture was heated at 85° C. for 16 hours. The reaction mixture was allowed to cool to room temperature, diluted with EtOAc (50 mL) and washed with H2O (50 mL×3). The organic layer was dried over sodium sulfate and concentrated. The resulting residue was purified by CombiFlash with 10% EtOAc in Hexane as the eluent to afford the desired 2-methyl-2-(2-nitro-phenylamino)-propionic acid tert-butyl ester (640 mg, 50%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09150556B2 |
|---|
| 出典データセット | uspto-grants-2015_10 |
|---|
| ORD ID | ord-a56a2960a3f54036a5b1cb5607203a81 |
|---|
| 出典メモ | uspto-grants-2015_10 |
|---|
