Dimethyl Sulfate → Vincamine methylsulfate

HRID 1112367

Reaktionsgleichung

Reaktionsgleichung von HRID 1112367
[CH3:1][CH2:2][C@:3]12[CH2:19][C@:18]([OH:24])([C:20]([O:22][CH3:23])=[O:21])[N:17]3[C:9]4=[C:10]([CH2:25][CH2:26][N:7]([C@@H:8]14)[CH2:6][CH2:5][CH2:4]2)[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=13.[CH3:27][O:28][S:29]([O:32]C)(=[O:31])=[O:30]>CC(C)=O>[CH3:1][CH2:2][C@:3]12[CH2:19][C@:18]([OH:24])([C:20]([O:22][CH3:23])=[O:21])[N:17]3[C:9]4=[C:10]([CH2:25][CH2:26][N:7]([C@@H:8]14)[CH2:6][CH2:5][CH2:4]2)[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=13.[CH3:27][O:28][S:29]([O-:32])(=[O:31])=[O:30]

Komponenten

4

Edukt 2

HCID 6497Dimethyl SulfateHCID 15376Vincamine

Produkt 1

HCID 86736090Vincamine methylsulfate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

7.08 g (2.10-2 moles) of vincamine are dissolved in 900 mls of boiling anhydrous acetone. Under stirring, 1.8 mls of dimethylsulfate are added and the resulting mixture is maintained under boiling for 6 hours. The mixture is concentrated to 400 mls and maintained on standing for a night. The mixture is filtered, washed onto the filter with ether and dried in a vacuum furnace at 50° C. There are obtained 7 g of a product having melting point of 191° C., soluble in water and alcohol.

Aufarbeitung

  1. temperaturethe resulting mixture is maintained
  2. concentrationThe mixture is concentrated to 400 mls
  3. temperaturemaintained
  4. waiton standing for a night
  5. filtrationThe mixture is filtered
  6. washwashed onto the
  7. filtrationfilter with ether
  8. customdried in a vacuum furnace at 50° C

Quellen und Nachweise

ORD-Eintrag
ord-9d3c0aeb99d14b63b3e3160bd9e958e9
Quelldatensatz
uspto-grants-1978_10
Patentnummer
US04122179

Verknüpfte Notizen

Wird geladen…