Piperazine → HCID 15230687, compound

HRID 892992

Reaction equation

HRID 892992 reaction equation
Cl[C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[N:5]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=2)[N:3]=1.[NH:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>C(O)C>[N:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[C:4]1[N:3]=[C:2]([N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[N:5]=1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 27670664-Chloro-2,6-di(2-pyridinyl)pyrimidine

Product 1

HCID 15230687HCID 15230687, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

4-Chloro-2,6-bis(2-pyridinyl)pyrimidine [prepared by the method of J.A.C.S. 32, 1591 (1967), 4.2 g] piperazine (13.44 g) and ethanol (70 ml) are heated at reflux for 2 hr. The mixture is allowed to cool and the solvent is removed under reduced pressure. The residue is dissolved in chloroform (250 ml), washed with water (twice), dried over sodium sulfate and concentrated under reduced pressure to give an oil. The oil is crystallized from ether to give the title compound, m.p. 159°-161°; MS (m/e) 318 (M+)

Workup

  1. temperatureat reflux for 2 hr
  2. temperatureto cool
  3. customthe solvent is removed under reduced pressure
  4. dissolutionThe residue is dissolved in chloroform (250 ml)
  5. washwashed with water (twice),
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto give an oil
  9. customThe oil is crystallized from ether

Sources & evidence

ORD record
ord-3590c6bde0314778b18b586b95e398af
Source dataset
uspto-grants-1992_06
Patent number
US05120843

Linked notes

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