Piperazine → HCID 15230687, compound

HRID 982527

Reaction equation

HRID 982527 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) is 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, mp 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-98a220d9cf1d4468af85217d0f49f0cb
Source dataset
uspto-grants-1991_02
Patent number
US04996318

Linked notes

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