Organic light emitting materials and devices
A technology of light-emitting devices and emitting materials, which is applied in the fields of light-emitting materials, organic chemistry, and electric solid devices, and can solve problems such as loss
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Embodiment 1
[0178] Step 1: Combine 3,5-bis(trifluoromethyl)phenylboronic acid (13.5 g, 52 mmol), 2-bromopyridine (6.2 g, 39 mmol), palladium(II) acetate (0.29 g, 1.3 mmol), tris Phenylphosphine (1.36 g, 5.2 mmol) and sodium carbonate (7 g, 68 mmol) were added to 200 mL of 1,2-dimethoxyethane and 100 mL of water. The reaction mixture was heated to reflux for 5 hours, and after cooling, 100 mL of water and 100 mL of ethyl acetate were added. The phases were separated, the organic layer was dried over magnesium sulfate and excess solvent was removed. 2-(3,5-bis(trifluoromethyl)phenyl)pyridine was purified by column chromatography and a white solid (7.1 g) was collected.
[0179] Step 2: 2-(3,5-Bis(trifluoromethyl)phenyl)pyridine (1.4 g, 4.8 mmol) from Step 1 above and iridium(III) chloride hydrate (0.87 g, 2.4 mmol) were added In a flask containing 15 mL of 2-methoxyethanol and 5 mL of water. The reaction mixture was heated to reflux for 16 hours and cooled. The yellow precipitate was co...
Embodiment 3
[0182] Step 1: 2,4-Difluoro-5-(trifluoromethyl)bromobenzene (2.0 g, 7.7 mmol), 2-tributylstannylpyridine and bis(triphenylphosphine)palladium(II) chloride (0.16 g, 0.23 mmol) was added to 50 mL of xylene and the mixture was heated to reflux for 16 hours. The reaction mixture was filtered through a plug of silica gel followed by purification by column chromatography to give 2-(2,4-difluoro-5-trifluoromethylphenyl)pyridine (1.4 g, 5.4 mmol). product by mass spectrometry and 1 Confirmed by H NMR.
[0183]Step 2: 2-(2,4-Difluoro-5-trifluoromethylphenyl)pyridine (1.4 g, 5.4 mmol) and iridium(III) chloride hydrate (0.97 g, 2.7 mmol) were added to 10 mL of 2- Methoxyethanol and 3 mL of water. The reaction mixture was heated for 16 hours and the pale green precipitate was collected by vacuum filtration and washed with water and hexanes. The dichloro bridged dimer was dried in a vacuum oven to give 1.0 g (50% yield). The product was used in the next step without purification.
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