関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N,N-Dimethylaniline | HCID 949 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Cyclopentylacetyl chloride | HCID 3485182 | — |
| 反応物 | 16beta-Ethyl-17beta-glycoloyloxy-4-estren-3-one | HCID 70466441 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 16beta-Ethyl-17beta-cyclopentylacetoxyacetoxy-4-estren-3-one | HCID 70467431 | — |
反応手順
In 10 ml of dichloromethane are dissolved 0.5 g of 16β-ethyl-17β-glycoloyloxy-4-estren-3-one and 0.2 ml of N,N-dimethylaniline and, with stirring, 0.3 ml of cyclopentylacetyl chloride is added. The mixture is stirred at room temperature (15°-25° C.) overnight and 150 ml of ethyl acetate is added. The mixture is washed with 10% H3PO4, water, 10% aqueous NaHCO3, water and saturated aqueous sodium chloride solution in that order and dried over anhydrous magnesium sulfate. The solvent is then distilled off and the residue is subjected to column chromatography. Following passage of 80 ml of diisopropyl ether-n-hexane (1:10), elution is carried out with 80 ml of a 1:1 mixture of the same solvents. The eluate is evaporated under reduced pressure to remove the solvent, giving 0.1 g of the above-identified compound as a colorless 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-a7eafb5a9e0f40e9a62afd5c8aa56723 |
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| 出典メモ | uspto-grants-1986_09 |
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