Method for synthesis of high purity trimethyl silicon based imidazole
A technology of trimethylsilyl imidazole and a synthesis method, which is applied in the directions of silicon organic compounds, sustainable manufacturing/processing, climate sustainability, etc. It can reduce the production of imidazole and silyl ether, shorten the reaction time, and simplify the process flow.
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[0013] Example 1
[0014] Add 34g (0.5mol) imidazole and 1.2g (0.002mol) magnesium stearate into a 250ml three-necked flask with a constant pressure dropping funnel, thermometer, magnetic stirring and 1 meter rectification column, and add 96.6g (0.6 mol) Hexamethyldisilazane is added to the constant pressure dropping funnel. Then heat, turn on the magnetic stirring, control the temperature of the reactor at about 140°C, slowly add hexamethyldisilazane dropwise from the constant pressure funnel, and rectify while reacting. The by-product ammonia gas is absorbed by water, and the distillation column The fraction below 105°C is collected at the top, and the reaction time is controlled to 2 hours. After the reaction, the reaction solution was subjected to vacuum distillation to obtain a high-content trimethylsilyl imidazole product with a yield of 88% and a content of 99.3%.
Example Embodiment
[0017] Example 3-8
[0018] Similar to Example 1, the reaction temperature was controlled to 140°C, the reaction time was 2 hours, and the type of stabilizer and the amount of catalyst were changed. The reaction results are as follows (Table 1):
[0019] Table 1 The effect of different types and dosages of stabilizers on the reaction
[0020]
Example Embodiment
[0021] Examples 9-15
[0022] Similar to Example 1, using zinc stearate as a stabilizer, the molar ratio of zinc stearate and imidazole is 0.001:1, and the molar ratio of hexamethyldisilazane and imidazole is 1.2:1. Change the reaction temperature, The conditions of reaction pressure and reaction time, the reaction results are as follows (Table 2):
[0023] Table 2 The influence of different reaction conditions on the reaction
[0024]
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