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Dichloromethane → (3beta)-3-[(1-Ethoxyethyl)oxy]pregn-5-en-20-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Pregnenolone | HCID 8955 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Ethyl vinyl ether | HCID 8023 | — |
| 生成物 | (3beta)-3-[(1-Ethoxyethyl)oxy]pregn-5-en-20-one | HCID 54547839 | — |
反応手順
—Pyridium p-toluenesulfonate (6.32 g) was added to a solution of (3β)-3-hydroxypregn-5-en-20-one (1; 100 g) in dichloromethane (600 ml) and ethyl vinyl ether (200 ml). After stirring of the reaction mixture for 1 h at room temperature triethylamine (20 ml) was added, whereupon the mixture was poured into a saturated aqueous solution of sodium hydrogen carbonate (1 l). The product was extracted into dichloromethane; the combined organic phases were washed with brine, dried over sodium sulfate, and concentrated under reduced pressure to give (3β)-3-[(1-ethoxyethyl)oxy]pregn-5-en-20-one (2; 125.6 g), which was used in the following step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06251887B1 |
| 出典データセット | uspto-grants-2001_06 |
| ORD ID | ord-961e77002bc44415953e0afe8929298c |
| 出典メモ | uspto-grants-2001_06 |