HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 17alpha-Ethynyl-17beta-hydroxy-6,16-dimethyleneandrosta-4-en-3-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | 17alpha-Ethynyl-17beta-hydroxy-6beta-(N-phenyl-N-ethylaminomethyl)-16-methyleneandrosta-4-en-3-one | HCID 13314926 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 17alpha-Ethynyl-17beta-hydroxy-6,16-dimethyleneandrosta-4-en-3-one | HCID 13314929 | — |
Reaktionsschritte
17α-Ethynyl-17β-hydroxy-6β-(N-phenyl-N-ethylaminomethyl)-16-methyleneandrosta-4-en-3-one (Example 5) 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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04526720 |
| Quelldatensatz | uspto-grants-1985_07 |
| ORD ID | ord-4f9918abd77142c49503c4720ebaec35 |
| Quellennotiz | uspto-grants-1985_07 |