Water → Stavudine

HRID 913266

Reaktionsgleichung

Reaktionsgleichung von HRID 913266
[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.O>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

4

Edukt 2

HCID 962WaterHCID 86625622Stavudine DMPU

Produkt 1

HCID 18283StavudineAusbeute 88,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
2.5 °C

Versuchsvorschrift

Stavudine-DMPU solvate (25 g, 0.07 moles), water (5 g) and isopropanol (250 ml) are heated to about 82° C. to get clear colorless solution. Heating is continued so as to distill the solution at atmospheric pressure until about 80 ml of isopropanol remained in side. The solution is allowed to cool on its own. The mixture is further cooled to 0-5° C. for 1.5 hrs. The precipitated product is filtered, washed with isopropanol (2×10 ml) and air dried to give 13.9 g (87.2%) of pure white crystalline Stavudine. The HPLC results are given in Table 2.

Aufarbeitung

  1. customto get clear colorless solution
  2. temperatureHeating
  3. distillationto distill the solution at atmospheric pressure until about 80 ml of isopropanol
  4. temperatureto cool on its own
  5. filtrationThe precipitated product is filtered
  6. washwashed with isopropanol (2×10 ml) and air
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-617fba8be3594a8fbcccd47e91e8e6a7
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08026356B2

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