Water → Di-[4-(2,2':6',2'')terpyridin-4'-yl-benzyl]-4,4'-azobis(4-cyanovalerate)

関与物質

反応手順

A reaction mixture of 4′-(4-bromomethylphenyl)-2,2′:6′,2″-terpyridine (1.500 g, 3.729 mmol), 4,4′-azobis(4-cyanopentanoic acid) (500 mg, 1.7839 mmol), Cs2CO3 (750 mg, 2.302 mmol), 1.0 ml of water and 100 ml of acetone was stirred vigorously at room temperature for 5 days. The solvents were removed under vacuum, and CH2Cl2 was added. The precipitate was filtered off. The filtrate was evaporated to dryness under vacuum, and then 300 ml of CH2Cl2-hexane mixture solvents (1:12, v/v) was added. The precipitate was filtered, and dried, and further purified by column chromatography (Al2O3) using ethyl acetate-hexane (3:2, v/v) as eluent to give pure product (0.763 g, 46%). 1H-NMR (CDCl3): δ=8.64 (m, 12H), 7.85 (m, 8H), 7.47 (m, 4H), 7.30 (m, 4H), 5.20 (s, 4H, —CH2—O—C(O)—), 2.65-2.48(m,8H, —OOC—CH2CH2—), 1.69(m, 6H, =N—C(CN)—CH3). HRMS (TOF): calculated for C56H47N10O4[(M+H)+] m/z=923.3782, found m/z=923.3759 Fluorescent Spectral Properties: λex=320 nm, λem=380 nm.

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