A kind of fluorenocarbazole derivative and its preparation method and application
A technology of fluorenocarbazole and derivatives, which is applied in the field of fluorenocarbazole derivatives and their preparation, and can solve problems such as difficult synthesis and constraints
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0048] Embodiment 1: the synthesis of intermediate fluorenocarbazole
[0049]
[0050] S1. In a 250mL three-necked flask, put 4-bromo-9,9-dimethyl-9H-fluorene (8.20g, 30mmol), 2-chloroaniline (4.59g, 36mmol), triphenylphosphine (0.04g , 0.15mmol), sodium tert-butoxide (8.65g, 90mmol), add 80mL ethanol and 40mL water, under nitrogen atmosphere, add tris(dibenzylideneacetone) dipalladium (0.27g, 0.3mmol), at 70°C Reaction 1-4h, liquid phase monitoring 4-bromo-9,9-dimethyl-9H-fluorene reaction is complete, add water to quench the reaction, separate liquid, concentrate the organic phase, rinse with petroleum ether through a silica gel column, rinse The solution was concentrated to obtain 9.02 g of N-(2-chlorophenyl)-9,9-dimethyl-9H-fluoren-4-amine as a colorless transparent oil, with a yield of 94% and a purity of 99.85%.
[0051] S2. In a 100mL three-necked flask, put the above-mentioned N-(2-chlorophenyl)-9,9-dimethyl-9H-fluorene-4-amine (5.67g, 20mmol), tri-tert-butylphosph...
Embodiment 2
[0052] Embodiment 2: the synthesis of compound (4)
[0053]
[0054] S3. In a 250mL three-necked flask, put the above-mentioned fluorenylcarbazole (4.25g, 15mmol), 5-bromo-2-iodopyridine (5.67g, 20mmol), 18-crown-6 (0.79g, 3mmol), Potassium carbonate (10.36g, 75mmol), add 75mL dimethylacetamide, under nitrogen atmosphere, add cuprous iodide (0.57g, 3mmol), react at 160°C for 4-8h, monitor the completion of the reaction in liquid phase, cool to room temperature, washed with water, filtered, and the filter cake was beaten again with 3-5 times of ethyl acetate, and then heated with a 10:1 ethyl acetate: ethanol mixed solvent to obtain white powdery intermediate 12-( 5-bromopyridin-2-yl)-fluorenocarbazole 5.47g, yield 83%.
[0055] S4. In a 100mL three-necked flask, put the above-mentioned intermediate 12-(5-bromopyridin-2-yl)-fluorenocarbazole (2.20g, 5mmol), 4,4-dimethyldiphenylamine (1.78g, 9mmol), tri-tert-butylphosphine tetrafluoroborate (0.06g, 0.2mmol), sodium tert-but...
Embodiment 3
[0057] Embodiment 3: the synthesis of compound (9)
[0058]
[0059] The 5-bromo-2-iodopyridine (5.67g, 20mmol) in Example 2 was replaced by 4-bromo-4'-iodo-1,1'-biphenyl (7.18g, 20mmol), 4,4-bis Methyldiphenylamine (1.78g, 9mmol) is replaced by diphenylamine (1.52g, 9mmol), and other synthetic processes are the same as in Example 2 (the intermediates of each corresponding step can be different, but other reactants, mol ratios, and reaction conditions are identical ) to obtain 2.50 g of compound (9) in the form of white powder, with a yield of 90%.
[0060] Mass spectrometer MALDI-TOF-MS (m / z) = 602.7803, theoretical molecular weight: 602.7810; Anal.Calcd forC 45 h 34 N 2 (%): C 89.67, H 5.69, N 4.65, Found: C 89.69, H 5.68, N 4.64.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 


