化工社化工社 化学情報印刷レポート · 研究参考用
Aluminum isopropoxide → 3-Methoxyestra-2,5(10)-dien-17-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aluminum isopropoxide | HCID 11143 | — |
| 反応物 | 3-Methoxyestra-2,5(10)-dien-17beta-ol | HCID 101963 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Cyclohexanone | HCID 7967 | — |
| 生成物 | 3-Methoxyestra-2,5(10)-dien-17-one | HCID 22791425 | 88.1% |
反応手順
Dissolve dl-3-methoxyestra-2,5(10)-dien-17β-ol (4 g) in cyclohexanone (40 ml) and toluene (140 ml) and add a solution of aluminum isopropoxide (4 g) in toluene (56 ml). Reflux in an atmosphere of nitrogen for two hours and cool. Add water (7.5 ml), shake, and then dry by adding sodium sulfate (10 g). Filter and evaporate under vacuum and recrystallize the residue from methanol to obtain dl-3-methoxyestra-2,5(10)-dien-17-one (3.5 g); m.p. 116°-118°; infrared absorption maxima at 5.76 μ, 5.9 μ, 6.01 μ.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03959322 |
| 出典データセット | uspto-grants-1976_05 |
| ORD ID | ord-b1399acfce7b47e09acec7d0d8711417 |
| 出典メモ | uspto-grants-1976_05 |