反应详情

49 g (94 mmol) of 6-(10-naphth-2-ylanthracen-9-yl)phenanthrene-9-carboxylic acid are suspended in 250 ml of quinoline, the suspension is saturated with N2, 11.8 g (38 mmol) of copper chromite are added, and the mixture is heated at the boil for 8 h. The mixture is subsequently poured into 1 l of MeOH/water, and the black solid is filtered off with suction, washed with MeOH and subjected to Soxhlet extraction with CHCl3. Removal of the solvent leaves a greyish solid, which is recrystallised four times from chlorobenzene and sublimed twice in vacuo (p=1×10−5 mbar, T=360° C.). The yield is 32 g (71%) with a purity>99.9%.

1. additionare added
2. temperaturethe mixture is heated at the boil for 8 h
3. filtrationthe black solid is filtered off with suction
4. washwashed with MeOH
5. extractionsubjected to Soxhlet extraction with CHCl3
6. customRemoval of the solvent
7. customleaves a greyish solid, which
8. customis recrystallised four times from chlorobenzene
9. customsublimed twice in vacuo (p=1×10−5 mbar, T=360° C.)