関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Glutaric anhydride | HCID 7940 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 16beta-Ethyl-17beta-glycoloyloxy-4-estren-3-one | HCID 70466441 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 16beta-Ethyl-17beta-(3-carboxypropyl)carbonyloxyacetoxy-4-estren-3-one | HCID 70467542 | 56.2% |
反応手順
In 10 ml of dimethylformamide is dissolved 0.5 g of 16β-ethyl-17β-glycoloyloxy-4-estren-3-one, and 0.2 g of glutaric anhydride and then 0.3 ml of triethylamine are added to the above solution. The mixture is allowed to stand at room temperature (15°-25° C.) for 3 hours and poured into 20 ml of 10% aqueous sulfuric acid, followed by extraction with 100 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography, elution being carried out with 200 ml of ethyl acetate. The eluate is evaporated under reduced pressure to remove the solvent, giving a colorless oil, which is allowed to stand to give 0.37 g of the above-identified compound as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04609650 |
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| 出典データセット | uspto-grants-1986_09 |
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| ORD ID | ord-8ad86bbd00414540bc192105b311a358 |
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| 出典メモ | uspto-grants-1986_09 |
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