Method for preparing paratoluensulfonyl chloride
A technology of p-toluenesulfonyl chloride and ammonium p-toluenesulfonate is applied in the field of preparation of p-toluenesulfonyl chloride, can solve the problems of unsafe use, difficult removal of phosphoric acid, complicated separation steps, etc., and achieves simple purification method, mild reaction conditions, The effect of convenient and easy-to-obtain raw materials
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Embodiment 1
[0029] The reactor is a three-necked flask with a volume of 250ml, equipped with a thermometer, mechanical stirring, reflux condenser and drying tube. 18.9 g of ammonium p-toluenesulfonate (100 mmol), 0.73 g of N,N-dimethylformamide (10 mmol) and 50 g of dichloroethane were added to the flask at one time. Start stirring, and at room temperature, the dichloroethane solution (which contains 10g triphosgene (34mmol), 50g of dichloroethane) dissolved with triphosgene is slowly and uniformly added dropwise to the reaction flask, and the dropping time is 30min. After adding, keep warm for 30min. After heat preservation, the temperature was raised until obvious reflux phenomenon appeared in the system, and the reaction was maintained under reflux conditions for three hours. After the reaction solution is cooled, the filter cake ammonium chloride is removed by filtration, and the obtained filtrate is subjected to vacuum distillation operation. After recovering 92g of dichloromethane,...
Embodiment 2～7
[0031] The type and amount of the organic base catalyst were changed, and other reaction conditions and raw material dosage were the same as in Example 1. The experimental results are shown in Table 1 below:
[0032] Table 1
[0033]
[0034]
[0035]As can be seen from the results in Table 1, the use of different types of organic amines as catalysts can obtain better experimental results, and if the amount of catalyst is large, the yield of p-toluenesulfonyl chloride is slightly higher, but there is no great impact on product purity.
Embodiment 8～13
[0037] Using N,N-diethylacetamide as the organic amine, changing the type and amount of solvent used in the reaction, distilling the filtrate after the reaction to recover 92% of the organic solvent, and then proceeding to the crystallization operation. Other reaction conditions and raw material charging amount are identical with embodiment 1. The experimental results are shown in Table 2 below:
[0038] Table 2
[0039]
[0040] As can be seen from the results in Table 2, the use of different types of inert organic solvents can obtain better experimental results, but when using chloroform as a solvent, the p-toluenesulfonyl chloride crystalline purity obtained is slightly lower, and is obtained in ethyl acetate and The product in petroleum ether has good crystallization performance and the obtained product has high purity.
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