化工社化工社 化学情報印刷レポート · 研究参考用
Formaldehyde → 3Betahydroxymethoxy-5-androsten-17-one acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Dehydroepiandrosterone | HCID 5881 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Chloromethyl acetate | HCID 69366 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3Betahydroxymethoxy-5-androsten-17-one acetate | HCID 131720566 | — |
反応手順
To a solution of dehydroepiandrosterone (2.88 g, 10 mmol) in THF (100 mL) is added sodium hydride (11 mmol, 60% in oil) at room temperature under an argon atmosphere. When all the sodium hydride has reacted, chloromethyl acetate (prepared from acetyl chloride and formaldehyde (or derivative) using ZnCl2 as catalyst) is added and the mixture is heated for a few hours. After cooling, the mixture is poured into water and extracted with ethyl acetate. The organic phase is then washed with water, dried, filtered and evaporated to dryness to give the desired compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728688 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-6642d755fcb048beb2e3a7e3e3b838c6 |
| 出典メモ | uspto-grants-1998_03 |