تفاعل #1256735

ord-5e97ec523bde47faacf2251994a41c68

معادلة التفاعل

[Na+].[OH-]
sodium hydroxide
CCCCCCCC/N=C(N)/N=C(\N)NCc1ccc(Cl)c(Cl)c1.Cl
olanexidine hydrochloride
CCCCCCCC/N=C(N)/N=C(\N)NCc1ccc(Cl)c(Cl)c1
olanexidine
المردود 87.8%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
25°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07825080B2uspto-grants-2010_11