4,7-Dichloro-1,10-phenanthroline

1,10-phenanthroline can be used as an intermediate in fluorescent materials, mainly in the fields of life sciences and medicine, catalysis, and novel optoelectronic materials.

Take 4.16g (10mmol) of 1,2-bis-[(2,2-dimethyl-4,6-dioxo-1,3-dioxane-5-ylidenemethyl)amino]benzene in 300mL of p-phenylene ether reflux for 30min, the mixture was cooled down to room temperature, when added to cyclohexane there was a large amount of precipitate precipitation precipitation, filtration and washed out of the p-phenylene ether with cyclohexane, vacuum drying to obtain 32.43g of light yellow powder crude The product was dried under vacuum to give 32.43g of light yellow powder crude product with a yield of about 99%. This product does not need to be purified, and can be directly carried out the next step of the reaction. Take 2.1g (10mmol) 4,7-dioxo-1,10-o-phenanthroline, add to 60g (210mmo1) phosphorus trichloride, under the protection of nitrogen reaction for 30min, the reaction solution was poured into 400mL of ice-water mixture, adjusted to pH 7-8 with 10% NaOH, extracted with dichloromethane (100mLx3), the organic layer was combined, dried with anhydrous magnesium sulfate, rotary evaporation with column chromatography. Drying, rotary evaporation and column chromatography gave 1.74 g of white powder product 4,7-dichloro-1,10-phenanthroline in 70% yield.