関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Bromophenol | HCID 7808 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Chloro-2,5-dimethyl-4-nitrobenzene | HCID 252793 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(4-Bromophenoxy)-2,5-dimethylnitrobenzene | HCID 68595356 | 68.8% |
反応手順
37.5 g (216.7 mmol) of 4-bromophenol and 35.4 g (256.2 mmol) of potassium carbonate are suspended in 500 ml of N,N-dimethylformamide and the suspension is stirred at room temperature for 1 h, before 36.6 g (197.0 mmol) of 4-chloro-2,5-dimethylnitrobenzene are added. The mixture is subsequently stirred at 150° C. for 14 h, water is added, and repeated extraction is carried out with ethyl acetate. The extracts are dried over Na2SO4 and filtered and the solvent is removed under reduced pressure. This is followed by purification by column chromatography (48.0 g, purity 91.0%, yield 68.8%, log P (pH 2.3)=4.86).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08748662B2 |
|---|
| 出典データセット | uspto-grants-2014_06 |
|---|
| ORD ID | ord-57c2386e089940c09c2e46307af27afd |
|---|
| 出典メモ | uspto-grants-2014_06 |
|---|
