Triphenylphosphine → HCID 21182289, compound

Participants

Reaction Steps

A solution of triphenylphosphine (3.46 g, 0.013 mol) and DEAD (2.30 g, 0.012 mol) in dry cold THF (100 ml) was added dropwise over 10 min to a solution of 4-bromo-4′-hydroxybiphenyl (3.00 g, 0.012 mol) and 4-bromo-4′-(6-hydroxyhexyloxy)biphenyl (2.20 g, 0.012 mol) (prepared as described in Example 4 step 2 above) in dry THF (50 ml) stirring at room temperature. The reaction mixture was left stirring overnight The reaction product was extracted into diethyl ether (2×200 ml), and the combined ethereal solutions were washed with water and dried (MgSO4). The crude product was adsorbed onto silica gel and purified by column chromatography [DCM-petroleum fraction (bp 40-60° C.), 1:6] and recrystallised from ethanol to give white crystals.

Provenance & Evidence