Reaktion #364147

ord-86526ee352614e32b5421feef0c1b86e

Reaktionsgleichung

O.O=C(O)CC(O)(CC(=O)O)C(=O)O
citric acid monohydrate
Clc1ccc(C2=CCN(CCCCn3cncn3)CC2)cc1
4-(4-chlorophenyl)-1,2,3,6-tetrahydro-1-[4-(1H-1,2,4-triazol-1-yl)butyl]pyridine
Clc1ccc(C2=CCN(CCCCn3cncn3)CC2)cc1.O=C(O)CC(O)(CC(=O)O)C(=O)O
4-(4-chlorophenyl)-1,2,3,6-tetrahydro-1-[4-(1H-1,2,4-triazol-1-yl)butyl]pyridine citrate
Ausbeute 84.6%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationwhich is filtered
  2. 2
    Waschenwashed with cold ethanol
  3. 3
    Sonstigedried

Vorschrift

A solution of citric acid monohydrate (33.8 g, 0.16 mol) in water (30 ml) is added to a solution of 4-(4-chlorophenyl)-1,2,3,6-tetrahydro-1-[4-(1H-1,2,4-triazol-1-yl)butyl]pyridine (51 g, 0.16 mol) in absolute ethanol (350 ml) at 40° C. After about 20 minutes a precipitate appears, which is filtered after cooling to room temperature, washed with cold ethanol and dried, yielding 68.9 g (84%) of 4-(4-chlorophenyl)-1,2,3,6-tetrahydro-1-[4-(1H-1,2,4-triazol-1-yl)butyl]pyridine citrate of m.p. 133-4° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06355659B1uspto-grants-2002_03