化工社化工社 化学情報印刷レポート · 研究参考用
Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester → (E)-3-(3-Chloro-benzo[b]thiophen-2-yl)-acrylic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester | HCID 17453 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3-Chloro-1-benzothiophene-2-carbaldehyde | HCID 818121 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (E)-3-(3-Chloro-benzo[b]thiophen-2-yl)-acrylic acid methyl ester | HCID 46825722 | — |
反応手順
A solution of 3.52 g (18.3 mmol) of 13 in 50 mL toluene was treated with methyl(triphenylphosphoranylidene)acetate (7.48 g, 21.9 mmol). After 4 h, saturated NaHCO3 solution (50 mL) was added and the mixture extracted with ethyl acetate (2×75 mL). The combined ethyl acetate solution was washed with brine (50 mL), dried (Na2SO4), filtered and evaporated. Purification by flash chromatography on silica gel (5% ethyl acetate/hexane) provided 3.60 g (14.6 mmol, 80%) of the enoate (14).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08754122B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-824feff9e81248b8b464da03e37175b7 |
| 出典メモ | uspto-grants-2014_06 |