HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium borohydride → 2Alpha,3alpha-epoxy-16beta-(1-pyrrolidinyl)-5alpha-androstan-17beta-OL
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium borohydride | HCID 4311764 | — |
| Edukt | (2a,3a,5a,16b)-2,3-Epoxy-16-(1-pyrrolidinyl)androstan-17-one | HCID 16063837 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2Alpha,3alpha-epoxy-16beta-(1-pyrrolidinyl)-5alpha-androstan-17beta-OL | HCID 16063872 | — |
Reaktionsschritte
After dissolving 39.2 g of 2α,3α-epoxy-16β-(1-pyrrolidinyl)-5α-androstan-17-one in a mixture of 392 ml of methanol and 56 ml of methylene chloride. 14.7 g Sodium borohydride are portionwise added while stirring and introducing nitrogen at such a rate that the temperature reaches room temperature as a maximum. The solution containing a precipitate is left to stand for 12 hours, then methylene chloride is evaporated, and the residue is diluted with water. The precipitate is filtered, thoroughly washed with water, dried and recrystallized from methanol to obtain the title product in a yield of 33.3 g (89.5%), m.p.: 167°-169° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05591735 |
| Quelldatensatz | uspto-grants-1997_01 |
| ORD ID | ord-0d678ac59c064668847b731576bd4390 |
| Quellennotiz | uspto-grants-1997_01 |