関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyltriphenylphosphonium iodide | HCID 638159 | — |
| 反応物 | 2-Fluoro-5-methoxybenzaldehyde | HCID 2734872 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Fluoro-4-methoxy-2-vinylbenzene | HCID 11446446 | 92.2% |
反応手順
39.4 g of methyltriphenylphosphonium iodide and 10.9 g of potassium t-butoxide were suspended in 150 ml of tetrahydrofuran. The resulting suspension was stirred at 0° C. under nitrogen stream for 30 minutes, followed by the dropwise addition thereto of a solution of 10 g of 2-fluoro-5-methoxybenzaldehyde in 20 ml of tetrahydrofuran. The resulting mixture was further stirred for one hour, quenched by the addition of water and extracted with ethyl acetate. The formed organic layer was washed with water and brine successively, dried over anhydrous magnesium sulfate, and evaporated. The resulting residue was subjected to silica gel column chromatography (developer: 5% ethyl acetate/n-hexane) to give 9.1 g of the title compound as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06358995B1 |
|---|
| 出典データセット | uspto-grants-2002_03 |
|---|
| ORD ID | ord-21d8b02e844649b2ac54108f4125b85c |
|---|
| 出典メモ | uspto-grants-2002_03 |
|---|