Chloroacetone → HCID 68744765, compound

HRID 2036181Notes

Reaction equation

HRID 2036181 reaction equation
[C:1]([N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:22][C:23](=[O:25])[CH3:24]>C(#N)C>[C:1]([N:9]1[CH2:14][CH2:13][N:12]([CH2:22][C:23](=[O:25])[CH3:24])[CH2:11][CH2:10]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 6571ChloroacetoneHCID 11430Potassium CarbonateHCID 7626541-Benzoylpiperazine

Product 1

HCID 68744765HCID 68744765, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

0.10 g (0.53 mmol) 1-benzoylpiperazine and potassium carbonate 0.22 g (1.58 mmol, 3.0 eq.) were added to 5 ml acetonitrile and 0.05 g (0.53 mmol, 1.0 eq.) chloroacetone was added dropwise slowly at room temperature. After mixing for one hour, 5 ml purified water was added, and the reaction mixture was extracted with 10 ml ethylacetate three times. After collecting organic layer, drying with anhydrous magnesium sulfate, and concentrating with decompression, residues obtained were purified with silicagel chromatography (mobile phase: dichloromethane/methnol=10:1) and 0.11 g (83%) target compound as yellow serup were yielded.

Workup

  1. additionwas added dropwise slowly at room temperature
  2. additionAfter mixing for one hour
  3. custom5 ml purified water
  4. additionwas added
  5. extractionthe reaction mixture was extracted with 10 ml ethylacetate three times
  6. customAfter collecting organic layer
  7. dry with materialdrying with anhydrous magnesium sulfate
  8. concentrationconcentrating with decompression, residues
  9. customobtained
  10. customwere purified with silicagel chromatography (mobile phase: dichloromethane/methnol=10:1) and 0.11 g (83%) target compound as yellow serup
  11. customwere yielded

Sources & evidence

ORD record
ord-6a3dc7d5310a436182ec655ff3faaf8a
Source dataset
uspto-grants-2013_11
Patent number
US08575173B2

Reaction notes

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