Method for preparing tetramethyl biphenyl
A technology for tetramethyl biphenyl and xylene, which is applied in the field of preparing tetramethyl biphenyl, can solve the problems of harsh conditions in the preparation process, increasing reaction steps and the like
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Embodiment 1
[0029] 1. Preparation of organic nickel catalyst:
[0030] R 1 is phenyl, R 2 For 2-fluorophenyl.
[0031] In a 100 ml three-necked flask, 0.61 g of salicylaldehyde and 0.55 g of o-fluoroaniline were dissolved in 30 ml of ethanol, and stirred at room temperature for 2 hours. Then 0.62 grams of nickel acetate tetrahydrate was dissolved in 10 milliliters of ethanol and added dropwise to the reaction flask, at which time the solution turned green. After continuing to stir for 4 hours, a solid precipitated out. The stirring was stopped and filtered to obtain 0.98 g of a green solid, which was then recrystallized with chloroform to obtain 0.88 g of a yellow-green solid with a yield of 90%.
[0032] Mass spectrum: 486, 272, 214, 195, 122, 95;
[0033] Elemental analysis: theoretical value: carbon 63.03%, hydrogen 3.83%, nitrogen 5.65%;
[0034] Measured values: carbon 62.83%, hydrogen 3.70%, nitrogen 5.64%;
Embodiment 2
[0036] 2. Synthesis of single spiro catalyst:
[0037] R 1 is phenyl, R 2 is 2,3,5,6-tetrafluoro-4-chlorophenyl, where Ph is phenyl.
[0038] Put 1 g of 2,3,5,6-tetrafluoro-4-chloroaniline and 0.61 g of salicylaldehyde into a 100 ml three-neck flask, add 30 ml of tetrahydrofuran, and then start stirring. During the stirring process, 6 grams of phenyl bis(triphenylphosphine) nickel chloride was added to the reaction flask in batches and stirred for 8 hours. After recrystallization of the obtained crude product with ethyl acetate and n-hexane, 3.66 grams of yellow-green Solid, 52.3% yield.
[0039] The X-ray single crystal diffraction data are shown in the attached figure figure 1 shown.
[0040] Molecular formula: C 37 h 25 CIF 4 NNiOP; molecular weight = 700.71
[0041] Crystal form: triclinic crystal
[0042]Spatial configuration: P-1, α=8.9835(11), b=13.1887(16), c=14.2291(16) , α=103.579(2), β=99.232(2), γ=99.500(2) °, V=1581.0(3) 3 , Z=2, μ=0.804mm -1 , Nu...
Embodiment 3
[0048] 3. Preparation of tetramethylbiphenyl from 4-chloro-o-xylene:
[0049] In a 250 ml three-necked flask, place 1.2 g of magnesium chips in 100 ml of n-butyl ether and stir vigorously, then at room temperature, start to slowly drop 7.1 g of 4-chloro-o-xylene, along with 4-chloro-o-xylene The instillation of magnesium chips gradually reduced. After the dropwise addition was completed, the temperature was raised to room temperature, and the stirring was continued. After about another 8 hours of reaction, the magnesium chips disappeared. Then in another 500 ml there-necked flask, under anhydrous, nitrogen protection 0 degree condition, the catalyst of 0.02 gram embodiment 1 and 7.1 gram of 4-bromo-o-xylene were dissolved in 100 milliliters of n-butyl ether, and then The Grignard reagent was slowly added dropwise into the reaction flask. After the dropwise addition, the temperature was raised to 75°C and stirred overnight. After stopping the reaction, the solution was poure...
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