Piperazine → HCID 15230687, Verbindung

HRID 982527

Reaktionsgleichung

Reaktionsgleichung von HRID 982527
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

Komponenten

4

Edukt 2

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

Produkt 1

HCID 15230687HCID 15230687, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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+).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-98a220d9cf1d4468af85217d0f49f0cb
Quelldatensatz
uspto-grants-1991_02
Patentnummer
US04996318

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