Method for synthesizing C-13 and C-14 labelled bisphenol A and C-13 and C-14 labelled tetrabromobisphenol A
A C-14, C-13 technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of long time and low efficiency of village wealth, and achieve the goal of increasing conversion rate and reducing cost. Effect
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Embodiment 1
[0029] Weigh 1.0 g 13 For C-phenol, add 0.5 ml of acetone and dissolve it in a 50 ml pear-shaped flask. In an ice bath, add 2.5 ml of 70% concentrated sulfuric acid dropwise (the volume ratio of acetone:concentrated sulfuric acid is 1:5). at 40 ° Reflux reaction at C for 15 min, when the reaction mixture turns from light yellow to yellow-brown, and solids are precipitated, take out the pear-shaped bottle, add about 15 ml of distilled water to dilute sulfuric acid in an ice bath to stop the reaction. Then 20 ml of dichloromethane was added to separate the organic and aqueous phases to remove the interference of acetone dissolving in the two phases. The lower organic phase was sucked out with a glass capillary pipette, and the extraction was repeated 3 more times. The extracted organic phase was dehydrated by anhydrous sodium sulfate, concentrated by rotary evaporation under reduced pressure, separated and purified by silica gel chromatography, the mobile phase was a mixed sol...
Embodiment 2
[0031] Embodiment 2, synthesis 13 C-bisphenol A and 13 C-Tetrabromobisphenol A
[0032] Weigh 0.3 g 13 For C-phenol, add 0.2 ml of acetone to dissolve in a 50 ml pear-shaped flask, and add 0.4 ml of 75% concentrated sulfuric acid dropwise in an ice bath (acetone:concentrated sulfuric acid = 1:2). at 45 °Reflux reaction at C for 10 min, when the reaction mixture turns from light yellow to yellow-brown, and solids are precipitated, take out the pear-shaped bottle, add about 15 ml of distilled water to dilute sulfuric acid in an ice bath to stop the reaction. Then 20 ml of dichloromethane was added to separate the organic and aqueous phases to remove the interference of acetone dissolving in the two phases. The lower organic phase was sucked out with a glass capillary pipette, and the extraction was repeated 3 more times. The extracted organic phase was dehydrated by anhydrous sodium sulfate, concentrated by rotary evaporation under reduced pressure, separated and purified b...
Embodiment 3
[0034] Embodiment 3, trace synthesis 14 C-bisphenol A and 14 C-Tetrabromobisphenol A
[0035] will be 1.83′ 10 8 Q 14 C-phenol (32 mg; 5.37′ 10 8 Bq / mmol), transferred to a 50 ml round bottom flask, added 1 ml acetone and a magnetic stir bar. In an ice bath, slowly add 600 μl of 73% concentrated sulfuric acid (acetone:concentrated sulfuric acid = 1:1) dropwise, while stirring quickly with a stirring bar to prevent the temperature of the system from rising. After the dropwise addition, close the bottle stopper tightly, at 50 ° Reflux reaction under C conditions for 10 min, when the reaction mixture turns from light yellow to yellow-brown, add 5 ml of distilled water to the flask in an ice bath to dilute sulfuric acid to stop the reaction. Then 10 ml of dichloromethane was added to separate the organic and aqueous phases to remove the interference of acetone dissolving in the two phases. The lower organic phase was sucked out with a glass capillary pipette, and the extr...
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