Reaction #2460332

Reaction equation

olanzapine

olanzapine

benzoic acid

benzoic acid

→

Olanzapine Benzoate

Solvents

ethyl acetate

ethyl acetate

Conditions

Workup

1. 1
   Other(T=50-55° C.)
2. 2
   workup.STIRRINGwhile stirring
3. 3
   OtherThe pale yellow crystals were isolated by filtration
4. 4
   Otherdried overnight at 40° C. in vacuum
5. 5
   OtherIsolated yield: 130.1 gram (94%)
6. 6
   Otherat 222.99° C.

Procedure

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.

Source