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p-Toluenesulfonic acid → HCID 10464631、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Ethyl vinyl ether | HCID 8023 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3-Carbethoxyumbeliferone | HCID 5289613 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 10464631 | HCID 10464631 | 26% |
反応手順
To a slurry of 5.0 g (21 mMol) of 3-carbethoxy-7-hydroxycoumarin [H. Pechmann and E. Graezer, Chem. Ber. 34:378(1901)] in 100 mL of CH2Cl2 containing 5 mL of ethylvinyl ether was added 30 mg of p-toluenesulfonic acid. After 15 minutes, the reaction was poured into 100 mL of 10% potassium hydroxide (KOH) solution. The organic phase was separated, washed with H2O, dried and evaporated. The residue was taken up in toluene and precipitated with hexane to give 1.73 g (26% yield) of the 1-ethoxyethyl ether as a solid, m.p. 70°-71° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04996332 |
| 出典データセット | uspto-grants-1991_02 |
| ORD ID | ord-90b9eeece987479fb772630df4ded897 |
| 出典メモ | uspto-grants-1991_02 |