Triethylamine → 5-Methoxy-2-piperazin-1-yl-pyrimidine hydrochloride

HRID 84764Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 84764
C(O[C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=O)(C)(C)C.[Cl:14]C1[N:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][N:16]=1.C(N(CC)CC)C>CN(C=O)C>[ClH:14].[CH3:22][O:21][C:18]1[CH:17]=[N:16][C:6]([N:8]2[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]2)=[N:20][CH:19]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 5890582-Chloro-5-methoxypyrimidine

Produkt 1

HCID 866866095-Methoxy-2-piperazin-1-yl-pyrimidine hydrochlorideAusbeute 51,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

1.5 g piperazine-1-carboxylic acid tert-butyl ester was added to 1.2 g 2-chlor-5-methoxy-pyrimidine and 2.2 mL triethylamine in 30 mL DMF. The reaction was stirred 6 days at 60° C. The solvent was removed and the residue was dissolved in dichlormethane and extracted with water. The organic layer was washed with a saturated sodiumchloride-solution and evaporated. The residue was purified by HPLC to give 957 mg desired product.

Aufarbeitung

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in dichlormethane
  3. extractionextracted with water
  4. washThe organic layer was washed with a saturated sodiumchloride-solution
  5. customevaporated
  6. customThe residue was purified by HPLC

Quellen und Nachweise

ORD-Eintrag
ord-ead407df16ec434db4c7c75237acbeef
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846948B2

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