関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| 反応物 | 4-Amino-3-Nitrophenol | HCID 3758882 | — |
| 反応物 | 4-chloro-N,N-dimethylpyridine-2-carboxamide | HCID 4962252 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(4-Amino-3-nitro-phenoxy)-pyridine-2-carboxylic acid dimethylamide | HCID 21037294 | — |
反応手順
A mixture containing 4-amino-3-nitrophenol (1 eq) and potassium bis(trimethylsilyl)amide (2 eq) was stirred in dimethylformamide for 2 hours at room temperature. To this mixture was added 4-Chloro-pyridine-2-carboxylic acid dimethylamide (1 eq) and potassium carbonate (1.2 eq) and then it was stirred at 90° C. for 3 days. The reaction mixture was then concentrated before partitioning between ethyl acetate and water. The organic layer was separated, washed with brine, dried, filtered and concentrated in vacuum to give brown solid. Purification by flash chromatography with ethyl acetate and hexane (1:1) gave the desired product as a yellow syrup. HPLC, 1.69 min; MS: MH+=303.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07728010B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-2ce32362d15346048dc575b0b0923ee7 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|