化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dichloroethane → 3,3,4,4,4-Pentafluorobutan-2-yl 4-formylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | 4-Formylbenzoic acid | HCID 12088 | — |
| 反応物 | 3,3,4,4,4-Pentafluorobutan-2-ol | HCID 78991 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3,3,4,4,4-Pentafluorobutan-2-yl 4-formylbenzoate | HCID 58930722 | 67% |
反応手順
A mixture of 4-carboxybenzaldehyde (21.9 g, 145.9 mmol), 3,3,4,4,4-pentafluoro-2-butanol (24.1 g, 146.9 mmol), EDC (33.5 g, 174.8 mmol) and DMAP (18.1 g, 148.1 mmol) was dissolved in DMF (60 ml) at rt. It was stirred for 36 h at rt. Hexane was added, it was washed with 1 N HCl, sat NaHCO3 and brine. The aqueous layers were extracted three times with hexane. It was dried over Na2SO4, filtered, concentrated, and the residue was purified by silica gel chromatography (ethyl acetate:hexane 1:10) to yield the desired aldehyde as a yellow oil (67%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07666902B2 |
| 出典データセット | uspto-grants-2010_02 |
| ORD ID | ord-98383c0ca2c24c1f9bb760a134a452a4 |
| 出典メモ | uspto-grants-2010_02 |