반응 #531789

반응 방정식

4,4′-(1,3-phenylene)bis(2,7,9-triphenyl-1,4,5,6-tetrahydro-1,10-phenanthroline-3-carbonitrile)

CH2Cl2

→

4,4′-(1,3-phenylene)bis(2,7,9-triphenyl-1,10-phenanthroline-3-carbonitrile)

용매

diethyleneglycol

반응 조건

후처리

1. 1
   온도was heated until total dissolution
2. 2
   온도the reaction was refluxed for 72 hours with argon bubbling directly in the solution

실험 절차

suspension of 4,4′-(1,3-phenylene)bis(2,7,9-triphenyl-1,4,5,6-tetrahydro-1,10-phenanthroline-3-carbonitrile) (5) in 2 L diethyleneglycol was heated until total dissolution. 10 g Pd/C was then slowly added, and the reaction was refluxed for 72 hours with argon bubbling directly in the solution. The reaction was monitored by TLC (Silica Gel; CH2Cl2). The starting material's spot (rf: 0.8, blue-green under 366 nm) converted into a blue fluorescent spot (rf: 0.9). Once the starting material spot has disappeared, the reaction was stopped, and the suspension cooled to room temperature.

출처