HCID 86625622, Verbindung → Stavudine

HRID 913262

Reaktionsgleichung

Reaktionsgleichung von HRID 913262
[CH3:1][C:2]1[C:8](=[O:9])[NH:7][C:5](=[O:6])[N:4]([C@@H:10]2[O:14][C@H:13]([CH2:15][OH:16])[CH:12]=[CH:11]2)[CH:3]=1.CN1C(=O)N(C)CCC1>C(O)(C)C>[C@@H:10]1([N:4]2[CH:3]=[C:2]([CH3:1])[C:8](=[O:9])[NH:7][C:5]2=[O:6])[O:14][C@H:13]([CH2:15][OH:16])[CH:12]=[CH:11]1

Komponenten

3

Edukt 1

HCID 86625622HCID 86625622, Verbindung

Produkt 1

HCID 18283StavudineAusbeute 98,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

Stavudine DMPU solvate (25 g, 0.060 mole) is dissolved in isopropanol (250 ml), and treated with activated carbon anti-eno crowns (2.5 g) at reflux temperature. Reaction mass is filtered while hot and washed with hot isopropanol (25 ml). The combined filtrate and wash are concentrated to 100 ml and allowed the mass to cool to room temperature slowly. Cooled the mass to 0-5° C. and the precipitated product is filtered. washed the product with chilled isopropanol (10 ml) and air dried to give 13.2 g (83%) of the title compound which purity greater than 99%. XRD data resembles crystalline form-I

Aufarbeitung

  1. additiontreated with activated carbon anti-eno crowns (2.5 g)
  2. temperatureat reflux temperature
  3. customReaction mass
  4. filtrationis filtered while hot and
  5. washwashed with hot isopropanol (25 ml)
  6. washThe combined filtrate and wash
  7. concentrationare concentrated to 100 ml
  8. temperatureCooled the mass to 0-5° C.
  9. filtrationthe precipitated product is filtered
  10. washwashed the product with chilled isopropanol (10 ml) and air
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-704beaa106dd4e47b01acf396000f4ad
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08026356B2

Verknüpfte Notizen

Wird geladen…