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Dimethylformamide → 16beta-Ethyl-17beta-(3,3-dimethylbutyryl)oxyacetoxy-4-estren-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | tert-Butylacetic acid | HCID 14057 | — |
| 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 | — |
| 生成物 | 16beta-Ethyl-17beta-(3,3-dimethylbutyryl)oxyacetoxy-4-estren-3-one | HCID 70467272 | 61% |
反応手順
In 10 ml of acetone is dissolved 1.16 g of 3,3-dimethylbutyric acid, and 5.0 ml of 2N-NaOH is added, followed by addition of 1.15 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 20 ml of DMF. The mixture is refluxed for 5 hours, and thereafter treated in the same manner as Example 26. The reaction mixture is chromatographed on a silica gel column. Following passage of 200 ml of n-hexanediisopropyl ether (3:7), elution is carried out with a 1:1 mixture of the same solvents. The eluate is evaporated under reduced pressure to remove the solvent, giving 0.76 g of the above-identified compound as a colorless viscous oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04609650 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-fc603816905c42dc89c27894771d8e96 |
| 出典メモ | uspto-grants-1986_09 |