1-Methylpiperazine → HCID 135815273, compound

HRID 1977634Notes

Reaction equation

HRID 1977634 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[CH3:8][N:9]1[C:17]2[C:16](=[O:18])[NH:15][C:14]([CH2:19][C:20]3[CH:25]=[CH:24][C:23]([S:26](Cl)(=[O:28])=[O:27])=[CH:22][CH:21]=3)=[N:13][C:12]=2[C:11]([CH2:30][CH2:31][CH3:32])=[N:10]1>C(O)C>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([S:26]([C:23]2[CH:24]=[CH:25][C:20]([CH2:19][C:14]3[NH:15][C:16](=[O:18])[C:17]4[N:9]([CH3:8])[N:10]=[C:11]([CH2:30][CH2:31][CH3:32])[C:12]=4[N:13]=3)=[CH:21][CH:22]=2)(=[O:27])=[O:28])[CH2:4][CH2:3]1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 135815255HCID 135815255, compound

Product 1

HCID 135815273HCID 135815273, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

N-methyl piperazine (1.28 ml, 0.0115 mol) was added to a solution of 4-[(1-methyl-7-oxo-3-propyl-6,7-dihydro-1H-pyrazolo[4,3-d]pyrimidin-5-yl)methyl]-1-benzenesulfonyl chloride (1.35 g, 0.0035 mol) in ethanol (20 ml) and the reaction stirred at room temperature for 18 hours. The reaction mixture was concentrated under reduced pressure and the residue partitioned between dichloromethane (50 ml) and water (20 ml). The aqueous phase was extracted with further dichloromethane (50 ml), the combined organic extracts dried (MgSO4), filtered, and evaporated under reduced pressure.

Workup

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue partitioned between dichloromethane (50 ml) and water (20 ml)
  3. extractionThe aqueous phase was extracted with further dichloromethane (50 ml)
  4. dry with materialthe combined organic extracts dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-05330c8dab2e496bacfff2ec6d88626c
Source dataset
uspto-grants-2001_05
Patent number
US06235742B1

Reaction notes

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