関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Iodotoluene | HCID 5128 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-(Phenylsulfonyl)ethanol | HCID 30202 | — |
| 反応物 | Tri-o-tolylphosphine | HCID 80271 | — |
| 反応物 | Methanesulfonic anhydride | HCID 81560 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-[2-(Benzenesulfonyl)ethenyl]-2-methylbenzene | HCID 70222490 | 81.3% |
反応手順
To 0.186 g (1.0 mmol) of 2-(phenylsulfonyl)ethanol, 3 ml of acetonitrile was added, followed by 0.19 g (1.1 mmol) of methanesulfonic anhydride and 0.56 ml (4.0 mmol) of triethylamine, and the mixture was stirred for 5 hours at the internal temperature of 50° C. Subsequently, 0.19 ml (1.5 mmol) of o-iodotoluene, 0.11 g (0.05 mmol) of palladium acetate, and 0.067 g (0.22 mmol) of tri(o-tolyl)phosphine were added thereto, and the mixture was then refluxed for 16 hours. After cooled to room temperature, the reaction mixture was concentrated and purified by column chromatography (hexane/ethyl acetate=80/20) to obtain 0.21 g of [2-(phenylsulfonyl)ethenyl]-2-methylbenzene. Yield: 80%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06201131B1 |
|---|
| 出典データセット | uspto-grants-2001_03 |
|---|
| ORD ID | ord-d48da67459714d2ab46cbc9130c61639 |
|---|
| 出典メモ | uspto-grants-2001_03 |
|---|