関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Heptanoic Acid | HCID 8094 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 16beta-Ethyl-17beta-bromoacetoxy-4-estren-3-one | HCID 15593764 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 16beta-Ethyl-17beta-n-heptanoyloxyacetoxy-4-estren-3-one | HCID 70467646 | 64% |
反応手順
In 30 ml of acetone is dissolved 2.6 g of n-heptanoic acid, and 10 ml of 2N-NaOH, 4.2 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one, 30 ml of DMF and 10 ml of water are serially added to the above solution. The mixture is refluxed for 5 hours. After cooling, 400 ml of ethyl acetate is added and the mixture is 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. Following 400 ml of diisopropyl ether-n-hexane (2:3), elution is carried out with 1000 ml of a 1:1 mixture of the same solvents. The eluate is evaporated under reduced pressure to remove the solvent, giving 3.0 g of the above-identified compound as a light-yellow viscous oil.
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-51711f58cf9043d294756a7ccce7d9b7 |
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| 出典メモ | uspto-grants-1986_09 |
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