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Hydrochloric Acid → 17alpha-Ethynyl-17beta-hydroxy-6,16-dimethyleneandrosta-4-en-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 17alpha-Ethynyl-17beta-hydroxy-6beta-(N-phenyl-N-ethylaminomethyl)-16-methyleneandrosta-4-en-3-one | HCID 13314926 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 17alpha-Ethynyl-17beta-hydroxy-6,16-dimethyleneandrosta-4-en-3-one | HCID 13314929 | — |
反応手順
17α-Ethynyl-17β-hydroxy-6-β-(N-phenyl-N-ethylaminomethyl)-16-methyleneandrosta-4-en-3-one (Example 3) in THF (20 ml) are mixed. Degassed hydrochloric acid (6N, 55 ml plus 20 ml THF) are added. The mixture is stirred overnight at 20°-25° under nitrogen, at which time TLC shows the reaction to be complete. Water (110 ml) is added, the mixture filtered, the solids washed with 10% hydrochloric acid, twice with water, once with 5% sodium bicarbonate, and three times with water to neutrality. Solids were then dried under nitrogen overnight to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04614621 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-84a0b588c67b42cf91f732ab7f5f1ccb |
| 出典メモ | uspto-grants-1986_09 |