Реакция #1256735

Уравнение реакции

sodium hydroxide

olanexidine hydrochloride

→

olanexidine

Выход 87.8%

Растворители

methanol

water

water

Условия реакции

Обработка

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

Методика

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.

Источник