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 | 3,4-Difluorobenzaldehyde | HCID 588088 | — |
| 反応物 | HCID 178418800 | HCID 178418800 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Fluoro-4-(4-methyl-1H-imidazol-1-yl)benzaldehyde | HCID 70700842 | 17.6% |
反応手順
4-Methylimidazole (46.4 g) and potassium carbonate (78.0 g) were added to a DMF solution (533 mL) of 3,4-difluorobenzaldehyde (40.0 g) at room temperature. This reaction solution was stirred at 90° C. for 6 hr and then was allowed to cool to room temperature. To the reaction solution, ethyl acetate and water were added. The organic layer was separated, washed with saturated saline, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluting solvent: heptane-ethyl acetate system) and further solidified with tert-butylmethylether to give 10.1 g of the title compound. The physical property values of this compound were as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07737141B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-c7bc762f2f1545c5a7b5de280b391cda |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|