Sodium Hydroxide → HCID 178443632, compound

HRID 2194341Notes

Reaction equation

HRID 2194341 reaction equation
[OH-].[Na+].[CH3:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10]/[N:11]=[C:12](/[N:14]=[C:15](/[NH:17][CH2:18][C:19]1[CH:20]=[CH:21][C:22]([Cl:26])=[C:23]([Cl:25])[CH:24]=1)\[NH2:16])\[NH2:13].Cl>O.CO>[CH3:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10]/[N:11]=[C:12](/[N:14]=[C:15](/[NH:17][CH2:18][C:19]1[CH:20]=[CH:21][C:22]([Cl:26])=[C:23]([Cl:25])[CH:24]=1)\[NH2:16])\[NH2:13]

Participants

5

Reactant 2

HCID 14798Sodium HydroxideHCID 178443633HCID 178443633, compound

Product 1

HCID 178443632HCID 178443632, compoundYield 87.8%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent2×

Conditions

Temperature
25 °C

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.

Workup

  1. customThe crystals obtained
  2. filtrationwere filtered off by suction filtration
  3. washwashed with water (500 mL)
  4. stirringThe suspension was stirred for 5 minutes at room temperature (approximately 25° C.)
  5. filtrationthe crystals were filtered off by suction filtration
  6. washwashed with water (500 mL)
  7. washThis operation (washing)
  8. customThe crystals obtained (wet weight: 127 g)
  9. waitThe resulting emulsion was left for 12 hours at room temperature
  10. customthe crystals precipitated
  11. filtrationwere filtered off by suction filtration
  12. customThe crystals were dried under reduced pressure at room temperature

Sources & evidence

ORD record
ord-03107f12e5d5460babeb86b7f3f036a5
Source dataset
uspto-grants-2012_12
Patent number
US08334248B2

Reaction notes

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