3,3',5,5'-TETRAMETHYLBIPHENYL synthesis
- Product Name:3,3',5,5'-TETRAMETHYLBIPHENYL
- CAS Number:25570-02-9
- Molecular formula:C16H18
- Molecular Weight:210.31
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Yield: 60%
Reaction Conditions:
with dipotassium hydrogenphosphate;palladium diacetate;silver carbonate in 1,2-dimethoxyethane at 150; for 12 h;Inert atmosphere;
Steps:
1 The preparation of the following formula 3,3',5,5'-tetramethylbiphenyl
In a 10 mL pressure-resistant reaction tube, 0.0300 g (0.2 mmol) of 2,4-dimethylbenzoic acid, 0.0045 g (0.02 mmol) palladium acetate, 0.0689 g (0.25 mmol) silver carbonate, 0.0087 g (0.05 mmol) dipotassium phosphate, 0.6 mL B Glycol dimethyl ether, under argon closed conditions, the reaction was stirred at 150 ° C for 12 hours, after the reaction was cooled to room temperature, Lee The mixture was filtered through a column of silica gel to remove salts and catalyst and was separated by thin-layer chromatography to give 3,3 ', 5,5'-tetramethylbiphenyl, which The yield is 60% and the structural characterization data is as follows:1H NMR (400 MHz, CDCl3): δ [ppm] = 7.19 (s, 4H), 6.97 (s, 2H), 2.3713C NMR (100 MHz, CDCl3): δ [ppm] = 141.5, 138.1, 128.7, 125.1, 21.4;GCMS (CI) m / z: Calculated for C16H18 [M] 210.14, Found 210.10.
References:
Shaanxi Normal University;Shi Xianying;Pu Fan;Liu Zhongwen CN107324964, 2017, A Location in patent:Paragraph 0014; 0015; 0016; 0017; 0018; 0019; 0020
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25570-02-9
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