Reacción #1256735

Ecuación de reacción

sodium hydroxide

olanexidine hydrochloride

→

olanexidine

Rendimiento 87.8%

Disolventes

methanol

water

water

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe crystals obtained
2. 2
   Filtraciónwere filtered off by suction filtration
3. 3
   Lavadowashed with water (500 mL)
4. 4
   workup.STIRRINGThe suspension was stirred for 5 minutes at room temperature (approximately 25° C.)
5. 5
   Filtraciónthe crystals were filtered off by suction filtration
6. 6
   Lavadowashed with water (500 mL)
7. 7
   LavadoThis operation (washing)
8. 8
   OtroThe crystals obtained (wet weight: 127 g)
9. 9
   workup.WAITThe resulting emulsion was left for 12 hours at room temperature
10. 10
    Otrothe crystals precipitated
11. 11
    Filtraciónwere filtered off by suction filtration
12. 12
    OtroThe crystals were dried under reduced pressure at room temperature

Procedimiento

A 4 N aqueous sodium hydroxide solution (120 mL) was added to a suspension of olanexidine hydrochloride (40 g) in water (360 mL), and the mixture was stirred for 90 minutes at 25° C. The crystals obtained were filtered off by suction filtration, washed with water (500 mL), and then resuspended in water (500 mL). The suspension was stirred for 5 minutes at room temperature (approximately 25° C.), and the crystals were filtered off by suction filtration, and then washed with water (500 mL). This operation (washing) was repeated once more. The crystals obtained (wet weight: 127 g) were dissolved in methanol (200 mL), and then water (60 mL) was added. The resulting emulsion was left for 12 hours at room temperature, and then the crystals precipitated were filtered off by suction filtration. The crystals were dried under reduced pressure at room temperature, whereby free olanexidine (32 g) was obtained.

Fuente