関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Bromo-5-methoxybenzaldehyde | HCID 344480 | — |
| 反応物 | 2,5-Difluorobenzene-1-thiol | HCID 3836323 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(2,5-Difluorophenylthio)-5-methoxy-benzaldehyde | HCID 12815952 | 52% |
反応手順
A mixture of 19.7 g of 2-bromo-5-methoxybenzaldehyde (of Example 9, reference above), 14.1 g of 2,5-difluorothiophenol (of Example 11, reference above), 14.0 g of potassium carbonate, 75 ml dimethylformamide and 2.1 g of copper catalyst is stirred and heated to 150° C. for 6 hours. It is then diluted with 150 ml of water and extracted with benzene. The extract is washed with water, dried with magnesium sulfate and evaporated. The residue is processed by distillation. There are obtained 13.3 g (52%) of 2-(2,5-difluorophenylthio)-5-methoxy-benzaldehyde boiling at 163°-165° C./40 Pa. The product is crystallized from cyclohexane and melts in a pure state at 67°-68° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04431808 |
|---|
| 出典データセット | uspto-grants-1984_02 |
|---|
| ORD ID | ord-0f3fefc692ba4cd192befc23e910e4a9 |
|---|
| 出典メモ | uspto-grants-1984_02 |
|---|