関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sulfur trioxide | HCID 24682 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | [3-(4-Benzyloxy-phenyl)-isoxazol-5-yl]-methanol | HCID 64164588 | — |
| 溶媒 | Dimethylsulfoxide-dichloromethane | HCID 21912085 | — |
| 生成物 | 3-(4-Benzyloxy-phenyl)-isoxazole-5-carbaldehyde | HCID 11818305 | — |
反応手順
[3-(4-benzyloxy-phenyl)-isoxazol-5-yl]-methanol (1.0 g, 3.5 mmol) was dissolved in 60 ml of DMSO/methylene chloride (1:2), to which solution were added dropwise sulfur trioxide.pyridine complex (1.6 g, 10.5 mmol) and triethylamine (2.44 ml, 17.5 mmol), and stirred at 0° C. for about 2 hours. The completion of the reaction was confirmed by TLC, and 10 ml of NH4Cl was added to the solution. The residual solvent was distilled under reduced pressure, and then extracted three times with water and methylene chloride. An organic layer was washed with saline solution. The obtained organic layer was distilled under reduced pressure, followed by column chromatography (ethyl acetate/Hexane=1:2) to obtain 3-(4-benzyloxy-phenyl)-isoxazol-5-carbaldehyde as a desired solid compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08828992B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-34655747a0874bf1ba2fad4898e979ab |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|