関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | HCID 15289161 | HCID 15289161 | — |
| 生成物 | 4,4-Dimethyl-2-(4'-methoxycarbonylbiphenyl-2-yl)oxazoline | HCID 15380877 | 91% |
反応手順
10.0 g (33.8 mmol) of 4,4-dimethyl-2-(4'-carboxybiphenyl-2-yl)oxazoline was dissolved in methylene chloride (200 ml). 4.8 g (40.3 mmol) of thionyl chloride was added thereto, followed by stirring at room temperature for 2 hours. The reaction liquid was subjected to vacuum concentration. Methanol (100 ml) was added to the residue, followed by stirring for 3 hours. After distilling out the solvent under a reduced pressure, methylene chloride and a saturated aqueous solution of sodium hydrogencarbonate were added to the residue and obtained mixture was caused liquid-liquid separation. After washing with water and drying, vacuum concentration was conducted. The residue was purified by silica gel column chromatography (an ethyl acetate/n-hexane system) to give 9.53 g of the title compound as an oil (yield 91%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05554757 |
|---|
| 出典データセット | uspto-grants-1996_09 |
|---|
| ORD ID | ord-be8a3c1f1c4644fbbc34e47b1141fb04 |
|---|
| 出典メモ | uspto-grants-1996_09 |
|---|