A kind of synthetic method of 2,6-dibromo-4-cyanophenol
A synthetic method, the technology of cyanophenol, applied in 2 fields, can solve the problems of poor environmental protection, low yield, complicated operation, etc., and achieve the effect of low cost, high product yield and simple steps
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Embodiment 1
[0021] Add 4g (0.034mol) of p-cyanophenol, 9.18g (0.034mol) of potassium persulfate and 7.6g (0.074mol) of sodium bromide into a 100mL round-bottomed flask, add 60mL of 50% ethanol aqueous solution, stir, and store at 50°C Reacted for 4 hours, after the reaction was over, filtered, washed the filter cake with water, and dried to obtain the product 2,6-dibromo-4-cyanophenol, which was a white solid with a yield of 92% and a purity of 98% by HPLC. Bruker AV-400 nuclear magnetic resonance spectrometer is used for nuclear magnetic resonance testing. The measurement conditions are: the separated and purified product is dissolved in deuterated chloroform for testing. The analysis results are: 1 H NMR (400MHz, CDCl 3 )δ 7.78(s, 2H), 6.38(s, 1H); 13 C NMR (100MHz, CDCl 3 )δ153.59, 135.65, 116.21, 110.41.106.55.
Embodiment 2
[0023] Add 4g (0.034mol) p-cyanophenol, 9g (0.037mol) sodium persulfate and 10.1g (0.085mol) potassium bromide to a 100mL round bottom flask, add 40mL of 50% methanol aqueous solution, stir, and irradiate under ultraviolet light React for 8 hours. After the reaction, filter, wash the filter cake with water, and dry to obtain the product 2,6-dibromo-4-cyanophenol, which is a white solid with a yield of 94% and a purity of 98% by HPLC.
Embodiment 3
[0025] Add 4g (0.034mol) p-cyanophenol, 31g (0.136mol) ammonium persulfate and 39g (0.272mol) cuprous bromide in 100mL round bottom flask, add N,N-dimethylformamide 80mL, stir, React at 30°C for 10 hours. After the reaction, filter, wash the filter cake with water, and dry to obtain the product 2,6-dibromo-4-cyanophenol, which is a white solid with a yield of 95.2% and an HPLC purity of 97.6%. .
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