Reacción #2460332

ord-6237dd45be50410bb32ecfa836607e1d

Ecuación de reacción

Cc1cc2c(s1)Nc1ccccc1N=C2N1CCN(C)CC1
olanzapine
Cc1cc2c(s1)Nc1ccccc1N=C2N1CCN(C)CC1
olanzapine
O=C(O)c1ccccc1
benzoic acid
O=C(O)c1ccccc1
benzoic acid
Cc1cc2c(s1)=Nc1ccccc1NC=2N1CCN(C)CC1.O=C(O)c1ccccc1
Olanzapine Benzoate

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otro(T=50-55° C.)
  2. 2
    workup.STIRRINGwhile stirring
  3. 3
    OtroThe pale yellow crystals were isolated by filtration
  4. 4
    Otrodried overnight at 40° C. in vacuum
  5. 5
    OtroIsolated yield: 130.1 gram (94%)
  6. 6
    Otroat 222.99° C.

Procedimiento

To a clear solution (50° C.) of 100 g olanzapine free base in 2000 ml ethyl acetate, was added slowly a clear solution of 39.2 g benzoic acid in 250 ml ethyl acetate while stirring mechanically. When almost all benzoic acid was added, the crystallization process started (T=50-55° C.). The mixture was allowed to cool to room temperature while stirring. The pale yellow crystals were isolated by filtration and dried overnight at 40° C. in vacuum. Isolated yield: 130.1 gram (94%). 1H-NMR confirms the molar ratio of olanzapine:acid=1:1. DSC: peak at 222.99° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07459449B2uspto-grants-2008_12