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Acetic Acid → [2-(4-Acetylamino-phenyl)-1,3-dihydroxy-indan-2-yl]-acetic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | [2-(4-Acetylamino-phenyl)-1,3-dioxo-indan-2-yl]-acetic acid ethyl ester | HCID 12776985 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | [2-(4-Acetylamino-phenyl)-1,3-dihydroxy-indan-2-yl]-acetic acid ethyl ester | HCID 69417565 | 17.3% |
反応手順
A stirred solution of [2-(4-acetylamino-phenyl)-1,3-dioxo-indan-2-yl]-acetic acid ethyl ester (4.0 g, Reference Example 13) in absolute ethanol (250 mL) was treated portionwise with sodium borohydride (1.7 g). After stirring at room temperature for 4 hours the reaction mixture was treated with glacial acetic acid until pH 7 and then evaporated. The residue was treated with water (100 mL) and the mixture was extracted with ethyl acetate (150 mL). The organic extract was dried over magnesium sulfate and then evaporated. The residue was subjected to chromatography on silica eluting with mixtures of dichloromethane and methanol (from 99.5:5 to 96:4, v/v) to give the title compound (0.7 g) as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07166616B2 |
| 出典データセット | uspto-grants-2007_01 |
| ORD ID | ord-4b6f96ec636940caa46e6f39b1ed9080 |
| 出典メモ | uspto-grants-2007_01 |