参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 硫代硫酸钠 | HCID 24477 | — |
| 反应物 | 4-叔丁基苯乙醇 | HCID 79410 | — |
| 反应物 | 戴斯-马丁氧化剂 | HCID 159087 | — |
| 溶剂 | 三氯甲烷 | HCID 6212 | — |
| 产物 | 4-叔丁基笨乙醛 | HCID 595340 | 80.2% |
反应步骤
A solution of 2-(4-tert-butylphenyl)ethanol (5.35 g, 30.0 mmol) in chloroform (150 mL) was cooled in ice and Dess-Martin periodinane (16.5 g, 39.0 mmol) was added thereto. The mixture was warmed to room temperature and stirred for 3 hr. The reaction mixture was diluted with chloroform (150 mL), followed by cooling in ice. Thereafter, saturated aqueous sodium thiosulfate solution was added thereto and the mixture was stirred for 5 min. The mixture was extracted three times with chloroform and then the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The desiccant was filtered off and then the filtrate was concentrated under reduced pressure. The resulting precipitate was filtered again, followed by washing with chloroform. The filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to afford the title compound as a yellow oil (4.24 g).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US09035059B2 |
|---|
| 来源数据集 | uspto-grants-2015_05 |
|---|
| ORD ID | ord-2074c7fe8f0340458aeb70fe936da491 |
|---|
| 来源说明 | uspto-grants-2015_05 |
|---|