反应详情

1.03 g (2.19 mmol) of perylene tetracarboxylic acid bis(allylimide) (compound (6), m=1, n=1) and 1.53 g (6.87 mmol) of 1,1,1,3,3,5,5-heptamethyl trisiloxane were dissolved in 100 ml of toluene, and 20 μl of a Karstedt catalyst (2 mol/l solution in xylene) was thereafter added thereto, which was then refluxed for 5 hours. The reaction solution thus obtained was then cooled and filtered, and the toluene was distilled off from a filtrate. The crude product thus obtained was purified by silica gel column chromatography (eluent: dichloromethane→dichloromethane-ethyl acetate (50:1)). The resultant crude product was dissolved in dichloromethane and re-precipitated with methanol. Thus, 1.51 g (1.65 mmol) of a red powder was obtained as an intended compound (1-1). A yield of the compound (1-1) was 75.3%. Values obtained by instrumental analysis of the compound (1-1) are shown below.

1. temperaturewhich was then refluxed for 5 hours
2. customThe reaction solution thus obtained
3. temperaturewas then cooled
4. filtrationfiltered
5. distillationthe toluene was distilled off from a filtrate
6. customThe crude product thus obtained
7. customwas purified by silica gel column chromatography (eluent: dichloromethane→dichloromethane-ethyl acetate (50:1))
8. dissolutionThe resultant crude product was dissolved in dichloromethane
9. customre-precipitated with methanol