Preparation method of 4-(4-dimethylaminostyryl)methylpyridyl p-toluenesulfonate
A technology of dimethylaminostyrene and p-toluenesulfonate, which is used in the preparation of 4-(4-dimethylaminostyryl)methylpyridine p-toluenesulfonate, and the preparation of high-quality organic nonlinear optics In the field of crystals, it can solve the problems of complicated synthesis steps, limited crystal growth, and long reaction time, and achieve the effects of simple preparation method, short reaction time, and simple reaction steps.
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[0018] The specific steps for preparing 4-(4-dimethylaminostyryl)picoline p-toluenesulfonate in this example include three steps: ion exchange reaction, condensation reaction, and filtration purification:
[0019] (1) Ion exchange reaction: at room temperature, mix 0.05mol 4-picoline (purity 98%) and 0.05mol methyl p-toluenesulfonate and place in 50-60ml anhydrous methanol (purity not less than 99.5 %), then mix the two solutions and put them in a 250ml three-hole flask, heat and stir slowly to 50°C, ion exchange reaction for 12-18h, and condense and reflux at the same time, the solution does not change color during the ion exchange reaction, and the reaction Obtain 4-methyl-N-methylpyridine p-toluenesulfonate;
[0020] (2) Condensation reaction: Weigh 0.05mol of p-dimethylaminobenzaldehyde (analytically pure) and dissolve it in 50-60ml of anhydrous methanol (purity not less than 99.5%), heat and stir until it is completely dissolved, Use a glass rod to drain and put it into ...
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