化工社化工社 化学情報印刷レポート · 研究参考用
Selenium Dioxide → Exemestane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Selenium Dioxide | HCID 24007 | — |
| 反応物 | 6-Methylideneandrost-4-ene-3,17-dione | HCID 12951800 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | Exemestane | HCID 60198 | 40.3% |
反応手順
A mixture of 6-methylenandrost-4-ene-3,17-dione (0.50 g), selenium dioxide (0.50 g) and t-butylalcohol (200 ml) was heated to reflux under nitrogen for about 30 hours. The cooled solution was filtered and then evaporated to dryness under reduced pressure. The residue was taken up in ethyl acetate (100 ml), treated with charcoal and washed consecutively with water, ammonium sulfide solution, cold 17% ammonium hydroxide, cold dilute hydrochloric acid, water, dried with sodium sulfate and finally evaporated to dryness. The crude product was chromatographed as described in example 1 to yield 0.20 g of pure 6-methylenandrosta-1,4-diene-3,17-dione, m.p. 188°-191° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04808616 |
| 出典データセット | uspto-grants-1989_02 |
| ORD ID | ord-ede5a1987d044f01a6811df98854f5b2 |
| 出典メモ | uspto-grants-1989_02 |