Reaction #1880944

ord-872eaaa3c77840f094de9da29bc6476f

Reaction equation

O=Cc1ccc[nH]1
pyrrole-2-carboxaldehyde
NCCN(CCN)CCN
tris(2-aminoethyl)amine
O.O=[N+]([O-])[O-].O=[N+]([O-])[O-].O=[N+]([O-])[O-].[Ga+3]
gallium(III) nitrate hydrate
NCCN=Cc1ccc[nH]1
[(((pyrrole-2-yl)methylidene)amino)ethyl]amine

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.STIRRINGstirred at room temperature for 30 min
  2. 2
    FiltrationThe solution was filtered
  3. 3
    workup.WAITleft
  4. 4
    Otherto stand at ambient temperature until crystallization
  5. 5
    Otherwas then sublimed at 235° C.

Procedure

The ligand [(((pyrrole-2-yl)methylidene)amino)ethyl]amine was prepared by adding a methanolic solution of pyrrole-2-carboxaldehyde (1.430 g, 15 mmol, 100 mL) to a methanolic solution of tris(2-aminoethyl)amine (0.720 g, 5 mmol, 10 mL). The resulting yellow solution was stirred at room temperature for 30 min. A methanolic solution of gallium(III) nitrate hydrate (1.280 g, 5 mmol, 150 mL) was added to the ligand solution and stirred at room temperature for 30 min. The solution was filtered and left to stand at ambient temperature until crystallization occurred. The crude material was then sublimed at 235° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07022421B2uspto-grants-2006_04