関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Hydroxybenzaldehyde | HCID 126 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | 3-Chloro-4-fluorobenzonitrile | HCID 145525 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Chloro-4-(4-formylphenoxy)benzonitrile | HCID 56851425 | 95% |
反応手順
Mix 4-hydroxy-benzaldehyde (0.86 g, 7.07 mmol), 3-chloro-4-fluoro-benzonitrile (1.00 g, 6.43 mmol), cesium carbonate (3.14 g, 9.64 mmol) and dimethylacetamide (30 mL) in a flask. Heat to 100° C. for 4 hrs. Let cool to room temperature (rt) and pour into water (200 mL). After trituration, filter the solid formed and dry on a vacuum pump to obtain the product (1.57 g, 95%). 1H NMR (DMSO-d6) 9.96 (s, 1H), 8.29 (d, J=1.8 Hz, 1H), 7.97 (d, J=8.6 Hz, 2H), 7.89 (dd, J=1.8 Hz, 8.6 Hz, 1H), 7.35 (d, J=8.6 Hz, 1H), 7.23 (d, J=8.6 Hz, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07381719B2 |
|---|
| 出典データセット | uspto-grants-2008_06 |
|---|
| ORD ID | ord-c6d3829e73514b4bb3288cb8de2dad08 |
|---|
| 出典メモ | uspto-grants-2008_06 |
|---|
