関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Fluorobenzonitrile | HCID 14517 | — |
| 反応物 | 2-Chloro-4-hydroxybenzaldehyde | HCID 185363 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(3-Chloro-4-formyl-phenoxy)-benzonitrile | HCID 49757377 | 14% |
反応手順
Dissolve 2-chloro-4-hydroxy-benzaldehyde (1.09 g, 7.01 mmol) in DMF (10 mL), add K2CO3 (1.06 g, 7.7 mmol) and 4-fluorobenzonitrile (932 mg, 7.7 mmol), heat the mixture at 130° C. overnight. Add water and extract the aqueous layer with EtOAc. Combine organic layers and dry over Na2SO4. Eliminate the solvent and purify by flash chromatography on silica gel (eluent: EtOAc/hexane 15/85) to give the title compound (240 mg, 14%), 1H-NMR (CDCl3, 300 MHz): 10.40 (s, 1H), 7.98 (d, 1H, J=8.6 Hz), 7.74-7.71 (m, 2H), 7.17-7.00 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07531557B2 |
|---|
| 出典データセット | uspto-grants-2009_05 |
|---|
| ORD ID | ord-936b6013748e4b08bf11266c5783d6e1 |
|---|
| 出典メモ | uspto-grants-2009_05 |
|---|
