Stavudine → Stavudine DMA

HRID 988754Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 988754
[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.[CH3:17][C:18]([N:20]([CH3:22])[CH3:21])=[O:19]>CC(C)=O>[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.[CH3:17][C:18]([N:20]([CH3:22])[CH3:21])=[O:19]

Komponenten

4

Edukt 2

HCID 18283StavudineHCID 31374Dimethylacetamide

Produkt 1

HCID 11722976Stavudine DMAAusbeute 78,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Reaktionsbedingungen

Temperatur
56 °C

Versuchsvorschrift

Crude white Stavudine (12.10 g, 94.25% pure, 0.0509 mole) was combined with DMA (18.15 g, 1.5 parts) and acetone (36 mL) and heated to 56° C. when all solids had dissolved. The cloudy mixture was filtered, distilled to remove acetone, cooled, filtered, washed with acetone and dried to give 12.35 g of white Stavudine-DMA solvate (0.0397 mole, 78.1%) with a chromatographic purity of 99.35%.

Aufarbeitung

  1. dissolutionhad dissolved
  2. filtrationThe cloudy mixture was filtered
  3. distillationdistilled
  4. customto remove acetone
  5. temperaturecooled
  6. filtrationfiltered
  7. washwashed with acetone
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2ab84db984f24d1f86eee921e540d3b1
Quelldatensatz
uspto-grants-2003_10
Patentnummer
US06635753B1

Notizen zur Reaktion

Wird geladen…