Triazabicyclodecene → HCID 86695684, Verbindung

HRID 335324

Reaktionsgleichung

Reaktionsgleichung von HRID 335324
[NH2:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[CH3:12])[C:5]([O:7]C)=O.N1CCCN2CCCN=C12.[CH3:23][N:24]1[CH2:29][CH2:28][N:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[CH2:36][NH2:37])[CH2:26][CH2:25]1>C1(C)C=CC=CC=1.CCOC(C)=O>[NH2:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[CH3:12])[C:5]([NH:37][CH2:36][C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=1[N:27]1[CH2:26][CH2:25][N:24]([CH3:23])[CH2:29][CH2:28]1)=[O:7]

Komponenten

6

Edukt 3

HCID 79873TriazabicyclodeceneHCID 337778Methyl 3-amino-4-methylbenzoateHCID 27955682-(4-Methyl-1-piperazinyl)benzenemethanamine

Produkt 1

HCID 86695684HCID 86695684, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A solution of methyl 3-amino-4-methylbenzoate (commercially available) (1.609 g, 9.74 mmol), TBD (2,3,4,6,7,8-hexahydro-1H-pyrimido[1,2-a]pyrimidine) (0.678 g, 4.87 mmol) and (2-(4-methylpiperazin-1-yl)phenyl)methanamine (commercially available) (2 g, 9.74 mmol) in toluene (30 ml) was heated at reflux overnight. The reaction mixture was diluted with EtOAc and washed with sat.NaHCO3 and water. The organic portion was separated, dried (MgSO4) and concentrated in vacuo. The product was purified by chromagraphy on silica eluting with a gradient of 0-20% 2M NH3 in MeOH/DCM to afford the title compound;

Aufarbeitung

  1. temperatureat reflux overnight
  2. washwashed
  3. customThe organic portion was separated
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe product was purified by chromagraphy on silica eluting with a gradient of 0-20% 2M NH3 in MeOH/DCM

Quellen und Nachweise

ORD-Eintrag
ord-71b9897385b34b5bb32f9468d007c604
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08883819B2

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