化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide → 2-Butyl-1-benzofuran-3-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 2-Butylbenzofuran | HCID 77951 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Butyl-1-benzofuran-3-carbaldehyde | HCID 4961966 | 74% |
反応手順
To a solution of DMF (59 g, 0.805 mol) in anhydrous DCM (300 mL) was added slowly at 0° C. under N2 atmosphere phosphorous oxy-chloride (123 g, 0.84 mol). The mixture was stirred at rt for 2 h. To this was added slowly 2-butyl-1-benzofuran (35 g, 0.21 mol) in anhydrous DCM (100 mL). The reaction mixture was slowly heated to 60° C. for 72 h, cooled to rt and poured into ice and extracted with EtOAc. The organic layer was washed with water, brine and dried over MgSO4. The solvent was removed under vacuum and the crude product purified by column chromatography over silica gel (PetEther/EtOAc) to give 2-butyl-1-benzofuran-3-carbaldehyde (30 g, 74%) as a light brown liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07592477B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-16efdabdfbd749c3a27507951c718c6a |
| 出典メモ | uspto-grants-2009_09 |