Benzo[lmn][3,8]phenanthroline-1,3,6,8(2H,7H)-tetrone,2,7-diphenyl- synthesis

Yield:24259-89-0 91.2%

Reaction Conditions:

with triethylamine in N,N-dimethyl-formamide at 130; for 1 h;Solvent;Temperature;

Steps:

1.1; 1.2; 1.3; 1.4; 1.5; 1.6; 1.7 Example 1

(1) 2 g of 1,4,5,8-naphthalene tetracarboxylic anhydride (NTCDA, 7.6 mmol)Was dissolved in 40.0 mL of dimethylformamide (DMF)Magnetic stir at 130 ;(2) Then, 2.1 mL of aniline (PA, 23.0 mmol) and4.3 mL triethylamine (30.0 mmol)Was added dropwise to the solution of step (1)Followed by magnetic stirring under reflux for 1 hour after a brown precipitate formed;(3) The mixed solution obtained in step (2) was centrifuged and filtered to remove the mother liquor to obtain a brown precipitate;(4) The resulting brown precipitate was dispersed in ethanol,And thoroughly cleaned with ethanol and then filtered to obtain a crude product soluble impurities;(5) and then the product obtained in step (4) was dissolved in dimethylformamide (DMF) and recrystallized to obtain an orange acicular recrystallized product;(6) The recrystallized product obtained in step (5) was washed with ethanol and filtered again;(7) The product obtained in step (6) was dried in a vacuum oven at 80 ° C. for 12 hours,2.9 g of the dried carbonyl conjugate heterocyclic compound N, N'-diphenyl-1,4,5,8-naphthalene diimide (DP-NTCDI) was weighed out in a yield of 91.2%.

References:

CN106518871,2017,A Location in patent:Paragraph 0020; 0027-0034; 0043-0050; 0053-0060