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1-Methylpiperazine → 1-[(N,N'-Di-p-tolyl)amidino]-4-methyl-piperizine

HRID 1813884
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1813884
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[C:8]1([CH3:24])[CH:13]=[CH:12][C:11]([N:14]=[C:15]=[N:16][C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)=[CH:10][CH:9]=1>CN(C=O)C>[C:8]1([CH3:24])[CH:13]=[CH:12][C:11]([NH:14][C:15]([N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]2)=[N:16][C:17]2[CH:18]=[CH:19][C:20]([CH3:23])=[CH:21][CH:22]=2)=[CH:10][CH:9]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 531671-MethylpiperazineHCID 69763Di-p-tolylcarbodiimide

Produkt 1

HCID 98836421-[(N,N'-Di-p-tolyl)amidino]-4-methyl-piperizineAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

1.05 mmol of 1-methylpiperazine was dissolved in 10 ml of N,N′-dimethylformamide (DMF), and 1.0 mmol of 1,3-di-p-tolylcarbodiimide was added. After 0.5 h. of stirring at room temperature, a small precipitation was removed by filtration and washed twice with 1 ml of DMF. The filtrates were collected and kept at room temperature overnight. 50 ml of water was added to the solution. An oil precipitated after 0.5 h which transformed into a solid. The solid residue was collected by filtration, washed twice with water and dissolved in 20 ml of methanol. 0.2 ml of conc. HCl was added was added to the methanol solution. After evaporation of the methanol, the residue was redissolved in methanol, and pure product was precipitated from the solution with ethyl ether. Yield=78%.

Aufarbeitung

  1. customa small precipitation
  2. customwas removed by filtration
  3. washwashed twice with 1 ml of DMF
  4. customThe filtrates were collected
  5. waitkept at room temperature overnight
  6. addition50 ml of water was added to the solution
  7. customAn oil precipitated after 0.5 h which
  8. filtrationThe solid residue was collected by filtration
  9. washwashed twice with water
  10. dissolutiondissolved in 20 ml of methanol
  11. addition0.2 ml of conc. HCl was added
  12. additionwas added to the methanol solution
  13. customAfter evaporation of the methanol
  14. dissolutionthe residue was redissolved in methanol
  15. custompure product was precipitated from the solution with ethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-9d916d402986456aaad4ee4eb054c539
Quelldatensatz
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06875759B1

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