Piperazine → HCID 3810979, compound

HRID 2230097Notes

Reaction equation

HRID 2230097 reaction equation
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[C:8]1[N:16]=[CH:15][N:14]=[C:13]2[C:9]=1[NH:10][CH:11]=[N:12]2>C(O)(C)C>[N:1]1([C:8]2[N:16]=[CH:15][N:14]=[C:13]3[C:9]=2[NH:10][CH:11]=[N:12]3)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 53592776-Chloropurine

Product 1

HCID 3810979HCID 3810979, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Procedure

To an isopropanol solution (50 mL) of piperazine (5.57 g, 64.7 mmol), 6-chloropurine (1.00 g, 6.47 mmol) was added, followed by stirring at room temperature for 1.5 hours and then heating under reflux for 2.5 hours. The reaction solution was concentrated, saturated brine was added thereto, the mixture was extracted with chloroform and THF in that order, the extract was dried over anhydrous sodium sulfate, and then the solvent was evaporated to give the target compound. Thereafter, the water layer after extraction was allowed to stand, and then the precipitated crystals were recovered by filtration to give the target compound (1.07 g in total, 5.25 mmol).

Workup

  1. temperatureheating
  2. temperatureunder reflux for 2.5 hours
  3. concentrationThe reaction solution was concentrated
  4. additionsaturated brine was added
  5. extractionthe mixture was extracted with chloroform and THF in that order
  6. dry with materialthe extract was dried over anhydrous sodium sulfate
  7. customthe solvent was evaporated
  8. customto give the target compound
  9. extractionThereafter, the water layer after extraction
  10. filtrationthe precipitated crystals were recovered by filtration
  11. customto give the target compound (1.07 g in total, 5.25 mmol)

Sources & evidence

ORD record
ord-e4cc29c3cdcb42e8a76e6d82f8fa0549
Source dataset
uspto-grants-2002_07
Patent number
US06423716B1

Reaction notes

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