4,5,9,10-Tetrabromobenzo[lmn][3,8]phenanthroline-1,3,6,8(2H,7H)-tetrone synthesis

Yield:943148-76-3 30%

Reaction Conditions:

with ammonium acetate;acetic acid for 2 h;Heating / reflux;

Steps:

10

Example 10; 2,3,6,7-Tetrabromonaphthalene-1,8;4,5-tetracarboximide; Naphthalene-1,4,5,8-tetracarboxylic acid (500 mg, 0.857 mmol) and ammonium acetate (1.32 g, 17.1 mmol) are heated to reflux with concentrated acetic acid to initially form a yellow solution. Later, an orange solid precipitates out, which is filtered off while hot after 2 h. The substance is washed with concentrated acetic acid (3 ml), water (5 ml), sat. sodium hydrogencarbonate solution (3 ml) and water again (5 ml), and then dried over phosphorus pentoxide.Yield: 150 mg (0.258 mmol, 30%)EI-MS: calc. for C₁₄H₂Br₄N₂O₄ [M]⁺: 581.7, found: 581.7m.p. >350° C.

References:

US2008/300405,2008,A1 Location in patent:Page/Page column 20