反应详情

In a 30 ml four-necked flask, 7.87 g (23.7 mM) of the p-pentadecanoxybenzaldehyde synthesized above and 8.65 g (11.0 mM) of p-xylylenebis(triphenylphosphonium bromide) were suspended in 100 ml of methanol, and 6.87 g (35.6 mM) of 28 wt % methylate was added thereto dropwise at room temperature (25° C.). The mixture was aged at a refluxing temperature of 65° C. for 3 hours. Methanol was removed by evaporation, and 200 ml of water was added to the residue, followed by stirring. The precipitate thus formed was collected by filtration, washed with water and acetone, and dried to give 7.49 g of a 1,4-bis(4′-pentadecanoxystyryl)benzene isomeric mixture (compound (1a)). The 1H-NMR data for identification were as follows.

1. addition6.87 g (35.6 mM) of 28 wt % methylate was added
2. customdropwise at room temperature
3. custom(25° C.)
4. customMethanol was removed by evaporation, and 200 ml of water
5. additionwas added to the residue
6. customThe precipitate thus formed
7. filtrationwas collected by filtration
8. washwashed with water and acetone
9. customdried