HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium borohydride → Npc182939
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium borohydride | HCID 4311764 | — |
| Edukt | Qing Hau Sau | HCID 9838675 | — |
| Edukt | Acetic acid methanol | HCID 10129899 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | Npc182939 | HCID 456410 | 75% |
Reaktionsschritte
Artemisinin (compound 3) (0.5 g, 1.8 mmole) in 40 mL of MeOH was cooled in an ice-bath to 0°-5° C. To the solution was added in small portions 0.25 g (6.6 mmole) of NaBH4 over a period of 30 minutes. The solution was stirred at 0°-5° C. for 2 hours after the addition of NaBH4 was complete. The solution was neutralized with 30% AcOH/MeOH and evaporated to dryness under reduced pressure. The white residue was extracted 3 times with 50 mL of EtOAc. The EtOAc extracts were combined, filtered, and evaporated to dryness to give 0.38 g (75%) of white needles mp 152°-154° C. (dec). Recrystallization from EtOAc-hexane raised the melting point to 153°-155° C. (lit. mp 153°-154° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04791135 |
| Quelldatensatz | uspto-grants-1988_12 |
| ORD ID | ord-42dfb6d64921409b843d06906f4bf799 |
| Quellennotiz | uspto-grants-1988_12 |