1-Methylpiperazine → HCID 178480770, Verbindung

HRID 1591579

Reaktionsgleichung

Reaktionsgleichung von HRID 1591579
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2[N:13]=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)[N:11]=[C:10]([OH:20])[CH:9]=2)[CH:3]=1.[CH3:21][N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1>CC(O)(CC)C.[Cl-].[Zn+2].[Cl-]>[CH3:21][N:22]1[CH2:27][CH2:26][N:25]([C:2]2[CH:7]=[CH:6][N:5]=[C:4]([C:8]3[N:13]=[C:12]([C:14]4[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=4)[N:11]=[C:10]([OH:20])[CH:9]=3)[CH:3]=2)[CH2:24][CH2:23]1

Komponenten

5

Edukt 2

HCID 531671-MethylpiperazineHCID 1785156306-(4-chloro-2-pyridinyl)-2-pyridin-2-yl-1H-pyrimidin-4-one

Produkt 1

HCID 178480770HCID 178480770, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3007855ZincchlorideKatalysatorHCID 64052-Methyl-2-butanolLösungsmittel

Versuchsvorschrift

A mixture of 3.51 g (12.3 mmol) of 6-(4-chloropyrid-2-yl)-2-pyrid-2-yl-pyrimidin-4-ol, 27.4 ml (303 mmol, 20 equivalents, 30.38 g) of 1-methyl-piperazine and 84 mg (0.05 mmol, 0.05 equivalent) of zinc(II) chloride in 50 ml of 2-methyl-2-butanol is refluxed for 22 hours and concentrated to dryness using a rotary evaporator. 50 ml of water are added, 3.6 g of EDTA are added, and the pH is adjusted to 9 using dilute sodium hydroxide solution. Extraction is carried out three times using 150 ml of chloroform each time, and the organic extracts are combined and dried (sodium sulfate). Concentration is carried out using a rotary evaporator and the crude product is recrystallised from toluene. 6-[4-(4-Methyl-piperazin-1-yl)-pyrid-2-yl]-2-pyrid-2-yl-pyrimidin-4-ol is obtained in the form of a whitish solid.

Aufarbeitung

  1. temperatureis refluxed for 22 hours
  2. concentrationconcentrated to dryness
  3. customa rotary evaporator
  4. addition50 ml of water are added
  5. addition3.6 g of EDTA are added
  6. extractionExtraction
  7. dry with materialdried (sodium sulfate)
  8. concentrationConcentration
  9. customa rotary evaporator
  10. customthe crude product is recrystallised from toluene

Quellen und Nachweise

ORD-Eintrag
ord-39eba654b162417ca0638b4a13f20a5a
Quelldatensatz
uspto-grants-2007_11
Patentnummer
US07291584B2

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