The Synthesis of Perylenebisimide Monocarboxylic Acids

✍ Scribed by Heinz Langhals; Wolfgang Lona

• Publisher: John Wiley and Sons
• Year: 1998
• Tongue: English
• Weight: 336 KB
• Volume: 1998
• Category: Article
• ISSN: 1434-193X
• DOI: 10.1002/(sici)1099-0690(199805)1998:5<847::aid-ejoc847>3.0.co;2-3

✦ Synopsis

mina (4 x 20 cm) and further purified by column separation. For this procedure, the dye was dispersed in acetic ester and added to the chromatographic column as well as the solid particles and eluted with acetic ester until nearly colourless. Then the dye is collected with chloroform/acetic acid (10 ϩ 1) which was evaporated. The residue was dissolved in a minimal amount of chloroform, filtered through a glass filter (D4), abundant distilled water was added and the chloroform was completely removed in vacuo. The solid was collected by vacuum filtration (D4 glass filter) and dried at 100°C with repeated pulverization in an agate mortar (because of the occlusion of water) until the solid became a fine, dry powder. This was further dried for 24 h in medium vacuum at 80°C to give 290 mg (60%) of 4a, m.p. > 350°C. Ϫ R f (silica gel, CHCl 3 /ethanol (10 ϩ 1)) ϭ 0.48. Ϫ R f (silica gel, CHCl 3 /acetic acid (10 ϩ 1)) ϭ 0.71. Ϫ IR (KBr): ν ˜ϭ 2955 cm Ϫ1 (m), 2926 (m), 2856 (m),