Piperazine → HCID 21916439, Verbindung

HRID 1246223Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1246223
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[C:8]1[N:13]=[C:12]([N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH:11]=[CH:10][N:9]=1>C(O)C>[CH2:17]([N:14]([CH2:15][CH3:16])[C:12]1[CH:11]=[CH:10][N:9]=[C:8]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[N:13]=1)[CH3:18]

Komponenten

4

Edukt 2

HCID 4837PiperazineHCID 126793942-chloro-4-(diethylamino)pyrimidine

Produkt 1

HCID 21916439HCID 21916439, VerbindungAusbeute 63,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of piperazine (5.8 g, 67.33 mmol) and N-(2-chloro-4-pyrimidinyl)-N,N-diethylamine (5.0 g, 26.93 mmol; preparation see: L. Strekowski, Pol. J. Chem. 1980, 54, 1557–62) in ethanol (200 ml) is heated at 100° C. for 16 hours. The mixture is then concentrated under reduced pressure and extracted with water/ethyl acetate. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulphate, filtered and concentrated under reduced pressure. Silica gel chromatography (mobile phase: dichloromethane/methanol) gives 4.01 g of the product (63%) as a yellow oil.

Aufarbeitung

  1. concentrationThe mixture is then concentrated under reduced pressure
  2. extractionextracted with water/ethyl acetate
  3. washThe organic phase is washed with saturated sodium chloride solution
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-f68ac8464b644acbbd3c2eeddc8c60ff
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07125995B2

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