関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methoxy-2-nitrobenzonitrile | HCID 288665 | — |
| 反応物 | Pyridinium chloride | HCID 10176127 | — |
| 生成物 | 4-Hydroxy-2-nitrobenzonitrile | HCID 53418121 | 26.5% |
反応手順
A mixture of 4-methoxy-2-nitrobenzonitrile (820 mg, 4.6 mmol) and pyridine hydrochloride (755 mg, 4.6 mmol) was heated at 200° C. under N2 for 18 hours. Upon completion, the reaction was cooled to room temperature, washed with brine and extracted with EtOAc (2×100 mL). The organic layers were combined, dried over MgSO4, filtered and concentrated. The residue was purified by flash chromatography (1:1 Hexane:EtOAc) to provide 4-hydroxy-2-nitrobenzonitrile (200 mg, 26%). 1H NMR (400 MHz, MeOD) δ 7.24 (dd, J=8.6, 2.4 Hz, 1H), 7.70 (d, J=2.4 Hz, 1H), 7.83 (d, J=8.6 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08633186B2 |
|---|
| 出典データセット | uspto-grants-2014_01 |
|---|
| ORD ID | ord-2e57716406dd41798765c53b1afdb0e0 |
|---|
| 出典メモ | uspto-grants-2014_01 |
|---|