Reaction #1256735

Reaction equation

sodium hydroxide

olanexidine hydrochloride

→

olanexidine

Yield 87.8%

Solvents

methanol

water

water

Conditions

Workup

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

Procedure

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.

Source