Stavudine DMA → Stavudine

HRID 988755

Reaktionsgleichung

Reaktionsgleichung von HRID 988755
[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.CC(N(C)C)=O>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

Komponenten

3

Edukt 1

HCID 11722976Stavudine DMA

Produkt 1

HCID 18283StavudineAusbeute 73,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

The Stavudine-DMA solvate (15.2 g, 0.0488 mole) was combined with water (15.2 g) and heated to 65° C. when all solids dissolved to give a clear colourless solution. The solution was allowed to cool on its own for an hour during which time a large amount of crystals formed. The mixture was cooled on an ice-water bath for 80 minutes, the crystals were crushed, filtered, washed with acetone and air dried to give 8.08 g (0.0360 mole, 73.7%) of pure white crystalline Stavudine. The HPLC results are given in Table 2.

Aufarbeitung

  1. dissolutiondissolved
  2. customto give a clear colourless solution
  3. temperatureto cool on its own for an hour during which time a large amount of crystals
  4. customformed
  5. temperatureThe mixture was cooled on an ice-water bath for 80 minutes
  6. customthe crystals were crushed
  7. filtrationfiltered
  8. washwashed with acetone and air
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-8d928977e43b4ddb820fdfce70668905
Quelldatensatz
uspto-grants-2003_10
Patentnummer
US06635753B1

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