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Potassium Carbonate → 1-(3-Chlorophenyl)-2-[2-(4-methylpiperazin-1-yl)ethoxy]ethanol dihydrochloride

HRID 862505
Notes
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Reaction equation

HRID 862505 reaction equation
C([O:4][CH:5]([C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([Cl:21])[CH:16]=1)[CH2:6][O:7][CH2:8][CH2:9]OS(C)(=O)=O)(=O)C.[CH3:22][N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1.C(=O)([O-])[O-].[K+].[K+].C[O-].[Na+]>CN(C)C=O.O.C(OCC)(=O)C.CO.C(OCC)C>[ClH:21].[ClH:21].[Cl:21][C:17]1[CH:16]=[C:15]([CH:5]([OH:4])[CH2:6][O:7][CH2:8][CH2:9][N:26]2[CH2:27][CH2:28][N:23]([CH3:22])[CH2:24][CH2:25]2)[CH:20]=[CH:19][CH:18]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

10

Reactant 4

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 10942334Sodium MethoxideHCID 536841961-Acetoxy-1-(3-chlorophenyl)-2-(2-methanesulfonyloxyethoxy)ethane

Product 1

HCID 675963491-(3-Chlorophenyl)-2-[2-(4-methylpiperazin-1-yl)ethoxy]ethanol dihydrochloride

Reagents, catalysts & solvents 5

HCID 887
Methanol
Solvent
HCID 962WaterSolvent
HCID 3283Diethyl EtherSolvent
HCID 6228DimethylformamideSolvent
HCID 8857Ethyl AcetateSolvent

Conditions

Temperature
80 °C

Procedure

1.40 g of 1-acetoxy-1-(3-chlorophenyl)-2-(2-methanesulfonyloxyethoxy)ethane was dissolved in 7 ml of N,N-dimethylformamide. To the solution were added 0.69 ml of N-methylpiperazine and 1.03 g of potassium carbonate. The mixture was stirred for 3 hours at 80° C. The reaction mixture was cooled and added to a mixture of 30 ml of ice water and 30 ml of diethyl ether. The organic layer was separated. The aqueous layer was extracted with 20 ml of diethyl ether. The extract was combined with the previously separated organic layer. The combined organic layer was washed with water and a saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue thus obtained was mixed with 7 ml of methanol and 45 mg of sodium methoxide. The mixture was allowed to stand overnight at room temperature. The solvent was removed by distillation under reduced pressure. To the residue thus obtained were added 20 ml of ethyl acetate and 10 ml of water. The organic layer was separated. The aqueous layer was extracted with 20 ml of ethyl acetate. The extract was combined with the previously separated organic layer. The combined organic layer was washed with a saturated aqueous sodium chloride solution and then purified by column chromatography (eluant: chloroform/methanol=10/1). To the resulting oily product were added 10 ml of ethanol and 1.2 ml of a 6N dry hydrogen chloride-ethanol solution in this order. To the resulting mixture was added 10 ml of diethyl ether. The mixture was stirred for 30 minutes. The resulting crystals were collected by filtration, washed with a mixture of 2 ml of ethanol and 2 ml of diethyl ether, and dried to obtain 770 mg of 1-(3-chlorophenyl)-2-[2-(4-methylpiperazin-1-yl)ethoxy]ethanol dihydrochloride (compound No. 158).

Workup

  1. temperatureThe reaction mixture was cooled
  2. customThe organic layer was separated
  3. extractionThe aqueous layer was extracted with 20 ml of diethyl ether
  4. washThe combined organic layer was washed with water
  5. dry with materiala saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate
  6. customThe solvent was removed by distillation under reduced pressure
  7. customThe residue thus obtained
  8. waitto stand overnight at room temperature
  9. customThe solvent was removed by distillation under reduced pressure
  10. customTo the residue thus obtained
  11. customThe organic layer was separated
  12. extractionThe aqueous layer was extracted with 20 ml of ethyl acetate
  13. washThe combined organic layer was washed with a saturated aqueous sodium chloride solution
  14. custompurified by column chromatography (eluant: chloroform/methanol=10/1)
  15. additionTo the resulting oily product were added 10 ml of ethanol and 1.2 ml of a 6N dry hydrogen chloride-ethanol solution in this order
  16. additionTo the resulting mixture was added 10 ml of diethyl ether
  17. stirringThe mixture was stirred for 30 minutes
  18. filtrationThe resulting crystals were collected by filtration
  19. washwashed with a mixture of 2 ml of ethanol and 2 ml of diethyl ether
  20. customdried

Sources & evidence

ORD record
ord-572ecf4ee8bc4a0baa70d949f1dc800a
Source dataset
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05719150

Reaction notes

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