化工社化工社 化学情報印刷レポート · 研究参考用
Benzene → 5-[2-(2,5-Dimethoxyphenyl)ethinyl]-2-hydroxybenzoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl 5-Iodosalicylate | HCID 248910 | — |
| 反応物 | 2,5-Dimethoxyphenylacetylene | HCID 11094951 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Oxygen | HCID 977 | — |
| 生成物 | 5-[2-(2,5-Dimethoxyphenyl)ethinyl]-2-hydroxybenzoic acid methyl ester | HCID 15384006 | — |
反応手順
Under argon atmosphere 240 mg of 2,5-dimethoxyphenylacetylene and 493 mg of methyl 5-iodosalicylate are dissolved in 20 ml of oxygen-free and dry benzene. The mixture is treated with 85 mg of tetrakis (triphenylphosphine)palladium, 20 mg of copper(I)iodide and 450 mg of triethylamine, stirred at room temperature overnight and then poured onto 100 ml of aqueous pH 7 buffer. After extraction with ethyl acetate and purification by chromatography on silicagel, 5-[2-(2,5-dimethoxyphenyl)ethinyl]-2-hydroxybenzoic acid methyl ester is obtained (colorless crystals of M.P. 105°-108°).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05488135 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-00b5aedde9b640c795ea84266ba6a003 |
| 出典メモ | uspto-grants-1996_01 |