関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-carboxylate | HCID 21703105 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(4-Fluorophenyl)-1,3-dihydroisobenzofuran-5-carboxylic acid | HCID 15538403 | 66% |
反応手順
Crude ethyl 1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-carboxylat (30 g) is dissolved in EtOH (96%, 150 ml) and aqueous 2N NaOH (150 ml). The solution is refluxed for 1 hour. ½ of the volume is removed in vacuo. The aqueous phase is extracted with EtOAc (2×100 ml). The aqueous phase is made acidic (pH=1, conc. HCl) and after cooling to 5° C. the white crystals are filtered off. Yield 16 g. Overall yield is 66% starting from 5-ethoxycarbonylphthalide. Mp 187-190° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06291689B1 |
|---|
| 出典データセット | uspto-grants-2001_09 |
|---|
| ORD ID | ord-972e933fb03a43018afe59087d33f334 |
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| 出典メモ | uspto-grants-2001_09 |
|---|
