Potassium Carbonate → HCID 86759067, compound

HRID 1296651Notes

Reaction equation

HRID 1296651 reaction equation
Cl[C:2]1[CH:7]=[N:6][CH:5]=[C:4]([Cl:8])[N:3]=1.[CH3:9][C@H:10]1[CH2:15][NH:14][C@H:13]([CH3:16])[CH2:12][NH:11]1.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[Cl:8][C:4]1[N:3]=[C:2]([N:11]2[CH2:12][C@@H:13]([CH3:16])[NH:14][CH2:15][C@@H:10]2[CH3:9])[CH:7]=[N:6][CH:5]=1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 785042,6-DichloropyrazineHCID 2206722,5-Dimethylpiperazine, trans-

Product 1

HCID 86759067HCID 86759067, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Conditions

Temperature
90 °C

Procedure

A mixture of 2,6-dichloropyrazine (0.40 g, 2.68 mmol), trans-2,5-dimethylpiperazine (0.62 g, 5.43 mmol), K2CO3 (0.41 g, 3.0 mmol) in acetonitrile (5 mL) was stirred at 90° C. for 6 h in a sealed pyrex tube. After cooling, the reaction mixture was filtered and concentrated in vacuo. The oily residue was purified by column chromatography on silica gel using CHCl3/MeOH (9:1) as eluent. This furnished 0.15 g (25%) of the title compound as an oil. HRMS m/z calcd for C10H15ClN4 (M)+ 226.0985, found 226.0983.

Workup

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtered
  3. concentrationconcentrated in vacuo
  4. customThe oily residue was purified by column chromatography on silica gel

Sources & evidence

ORD record
ord-eb81fc0fe8934e448dee52f942c7fe0a
Source dataset
uspto-grants-2007_07
Patent number
US07247633B2

Reaction notes

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