反応 #1880944

ord-872eaaa3c77840f094de9da29bc6476f

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGstirred at room temperature for 30 min
  2. 2
    ろ過The solution was filtered
  3. 3
    workup.WAITleft
  4. 4
    その他to stand at ambient temperature until crystallization
  5. 5
    その他was then sublimed at 235° C.

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07022421B2uspto-grants-2006_04