반응 #1256735

반응 방정식

sodium hydroxide

olanexidine hydrochloride

→

olanexidine

수율 87.8%

용매

methanol

water

water

반응 조건

후처리

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

실험 절차

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.

출처