化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 5alpha-Pregn-2-en-20-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3alpha-Toluene-p-sulphonyloxy-5alpha-pregnan-20-one | HCID 53885237 | — |
| 溶媒 | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| 生成物 | 5alpha-Pregn-2-en-20-one | HCID 246883 | 97% |
反応手順
The crude product 3α-toluene-p-sulphonyloxy-5α-pregnan-20-one in 30 mL of collidine was refluxed for 1.0 h. The solution was allowed to cool and then poured into cold dilute hydrochloric acid (200 mL) and extracted three times with CH2Cl2 (100 mL portions). The combined organic phase was dried over magnesium sulfate and concentrated. Flash chromatography on a silica gel bed (100 g) and elution with hexane/ethyl acetate (80:20) gave 4.65 g (97% yield for the two steps) of 5α-pregn-2-ene-20-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05591733 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-353428eb7881432f849ffb17c593adff |
| 出典メモ | uspto-grants-1997_01 |