Dimethylformamide → HCID 18976943, compound

Participants

Reaction Steps

In a 1 L three-hole flask equipped with a stirrer, a thermometer and a reflux condenser, 24.9 g (0.05 mol) of 2,7-bis(bromomethyl)-9-{2-[2-(2-methoxyethoxy)ethoxy]ethyl}fluorene, 39.3 g (0.15 mol) of triphenylphosphine, and 300 ml of dimethylformamide were introduced and reacted for 12 hours at reflux temperature. After reaction, the temperature was decreased to room temperature, and the reactant was dropped down slowly in 1.5 L of ethylether solvent under agitation, to obtain a white solid. After filtering, such extracted solid was washed several times with ethylether, and then dried sufficiently in a vacuum oven at 40° C. As a result, 48.5 g (yield: 95%) of a white solid was obtained. [1H=NMR (CDCl3), δ 1.22-1.41(m, 2H, CH2), 2.16-2.42(br, s, 3H, OCH3), 3.41-3.71(m, 10H, OCH2 CH2), 4.18(t, 1H, CH), 5.58-5.81(d, 4H, CH2Br), 6.81-7.22(m, 6H, fluoreyl aromatic), 7.27-7.84(m, 30H, aromatic)].

Provenance & Evidence