Method for synthesizing arylsulfonyl chloride
A technology of arylsulfonyl chloride and its synthesis method, which is applied in the direction of sulfonic acid preparation, organic chemistry, etc., can solve the problems of affecting product quality, inconvenient use, difficult to remove, etc., and achieve less waste, mild reaction conditions, and high product yield. The effect of high purity
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Embodiment 1
[0019] In a 50ml four-necked flask equipped with a thermometer, mechanical stirring, co-current condenser, drying tube and tail gas absorption bottle, add 3.38g (15mmol) sodium 2-nitrobenzenesulfonate, 0.065g (0.75mmol) N, N -Dimethylacetamide and 15ml 1,2-dichloroethane, start stirring, at room temperature, add dropwise 15ml of 1.78g (6.0mmol) bis(trichloromethyl) carbonate in 20 minutes 1, 2-dichloroethane solution. The temperature was raised to 83° C. under stirring, and the reflux reaction was maintained for 3 hours until no more gas was generated. After the reaction solution was cooled, the filter cake sodium chloride was removed by filtration, and the filtrate was distilled under reduced pressure to recover 1,2-dichloroethane, and the residue was recrystallized with petroleum ether to obtain 2.93 g of pure 2-nitrobenzenesulfonyl chloride. The yield is 85.6%, the purity is 97.2%, the appearance is light yellow crystalline powder, m.p.65~67℃ (literature value 67~68℃).
Embodiment 2
[0021] In a 50ml four-neck flask equipped with a thermometer, mechanical stirring, reflux condenser, drying tube and tail gas absorption bottle, add 2.7g (15mmol) sodium benzenesulfonate, 0.065g (0.75mmol) N,N-dimethylethane Amide and 15ml 1,2-dichloroethane, start stirring, at room temperature, dropwise add 1.78g (6.0mmol) bis(trichloromethyl)carbonate in 15ml 1,2-dichloroethane within 20 minutes alkane solution. The temperature was raised to 83° C. under stirring, and the reflux reaction was maintained for 3 hours until no more gas was generated. After the reaction solution was cooled, the filter cake sodium chloride was removed by filtration, and the filtrate was distilled under reduced pressure to recover 1,2-dichloroethane, and the residue was subjected to fractional distillation under reduced pressure to obtain 2.44 g of pure benzenesulfonyl chloride, with a yield of 90.4%. It is 98.1%, the appearance is colorless liquid, b.p.112~115℃ / 10mmHg (literature value 113~115℃ / 1...
Embodiment 3～8
[0023] The 2-nitrobenzenesulfonate sodium is replaced by the corresponding sodium arylsulfonate in the following table 1, the charging amount of all sodium arylsulfonates is 15mmol, and other operating conditions are all the same as in Example 1, and the obtained arylsulfonate The results of sulfonyl chloride are shown in Table 1.
[0024] Table 1
[0025]
PUM
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