化工社化工社 化学情報印刷レポート · 研究参考用
tert-Butanol → beta-Methylenephenethyl alcohol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butanol | HCID 6386 | — |
| 反応物 | Alpha-Methylstyrene | HCID 7407 | — |
| 反応物 | Decane | HCID 15600 | — |
| 反応物 | Selenium Dioxide | HCID 24007 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | beta-Methylenephenethyl alcohol | HCID 80106 | 59% |
反応手順
A 12.5 ml of decane solution of 5 to 6 mol/L of per-tert-butylalcohol is diluted with 50 ml of methylene chloride, then 111 mg of selenium dioxide and 90.1 mg of an acetic acid were added thereto to react while stirring at room temperature for 30 min. Then, 6.5 ml of 2-phenylpropene was added to the reaction solution to react while stirring for 72 hours, followed by condensation under reduced pressure, and purification by silica gel column chromatography to obtain 3.98 g of 3-hydroxy-2-phenylpropene (yield: 59%). Measurement results by 1H-NMR and 13C-NMR of 3-hydroxy-2-phenylpropene obtained are shown below.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741242B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-19597bdefb3548119f1a52e9b0ae7935 |
| 出典メモ | uspto-grants-2010_06 |