Nitrogen → Bis[4-(3-ethynylphenoxy)phenyl]methanone

Participants

Reaction Steps

In 20 ml of triethylamine, dissolved are 1.4 g (2.7 mmol) of 4,4'-bis(3-bromophenoxy)benzophenone and 0.67 g (8 mmol) of 2-methyl-3 -butyne-2-ol. Through this reaction mixture, N2 gas was allowed to flow for 20 min. To the resultant, 0.02 g of triphenylphosphine, 0.005 g of a palladium catalyst, i.e. (Ph3P)2PdCl2, and 0.005 g of copper iodide were added and reacted at 80° C. for 20 hours. The reaction mixture was then washed with water and subjected to extraction with methylenechloride. A intermediate reaction product was obtained by removal of the methylenechloride. To this intermediate reaction product, 20 ml of toluene, 10 ml of methanol, and 0.8 g of NaOH were added, and subsequently, the methanol and a portion of the toluene were distilled off at a temperature of 100° C. The resultant was then washed with water and subjected to extraction with methylenechloride. Finally, the extracting solvent was removed to obtain 1.3 g of 4,4'-bis(3-ethynylphenoxy) benzophenone. The yield was approximately 94%. The following is the reaction formula of this synthesis. ##STR8##

Provenance & Evidence