Stavudine → Stavudine DMPU

HRID 913264

Reaktionsgleichung

Reaktionsgleichung von HRID 913264
[C@@H:1]1([N:8]2[CH:16]=[C:14]([CH3:15])[C:12](=[O:13])[NH:11][C:9]2=[O:10])[O:7][C@H:4]([CH2:5][OH:6])[CH:3]=[CH:2]1.[CH3:17][N:18]1[C:23](=[O:24])[N:22]([CH3:25])[CH2:21][CH2:20][CH2:19]1>CC(C)=O>[CH3:15][C:14]1[C:12](=[O:13])[NH:11][C:9](=[O:10])[N:8]([C@@H:1]2[O:7][C@H:4]([CH2:5][OH:6])[CH:3]=[CH:2]2)[CH:16]=1.[CH3:17][N:18]1[C:23](=[O:24])[N:22]([CH3:25])[CH2:21][CH2:20][CH2:19]1

Komponenten

4

Edukt 2

HCID 18283StavudineHCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-

Produkt 1

HCID 86625622Stavudine DMPUAusbeute 87,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Reaktionsbedingungen

Temperatur
56 °C

Versuchsvorschrift

Crude Stavudine (25 g, 97.7% pure, 0.1116 mole), DMPU (37.5 g, 1.5 parts) are added to acetone (50 ml) and heated to 56° C. for dissolution. The obtained solution is stirred for 15 min. at 56° C. and cooled to 6-8° C. The precipitated product is filtered, washed with acetone and dried to give 34.4 g of Stavudine DMPU solvate (87.5%) with a chromatographic purity 99.93%.

Aufarbeitung

  1. temperaturecooled to 6-8° C
  2. filtrationThe precipitated product is filtered
  3. washwashed with acetone
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2bdc41f217664607a37266af142ffb4a
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08026356B2

Verknüpfte Notizen

Wird geladen…