Method for preparing high-purity cis-5-norbornene-exo-2,3-dicarboxylic anhydride through microwave reaction
A microwave reaction and norbornene technology, applied in the direction of organic chemistry, can solve the problems of complicated operation, low translocation yield, high toxicity of additives, etc., and achieve the effects of simple reaction process, short reaction time and few by-products.
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Embodiment 1
[0031] A method for preparing high-purity cis-5-norbornene-exo-2,3-dicarboxylic anhydride by microwave reaction, using cis-5-norbornene-inner-2,3-dicarboxylic anhydride as raw material, Specific steps are as follows:
[0032] (1) In a 1L reaction flask, stir 100g of cis-5-norbornene-endo-2,3-dicarboxylic acid anhydride and 100mL of xylene evenly, put it into a microwave reaction kettle, raise the temperature to 180°C, and Microwave reaction under 0.3-10GHz microwave for 5 minutes;
[0033] (2) After the reaction is completed, cool the reactor in step (1) to 90°C, place it in an oil bath and stir for 30 minutes to crystallize, cool to room temperature, filter, and dry to obtain the product cis-5-norbornene-exo Type-2,3-dicarboxylic acid anhydride 70.2g; yield: 70.2%; purity: 98.6%; oxide impurity content: 0.05%.
Embodiment 2
[0035] A method for preparing high-purity cis-5-norbornene-exo-2,3-dicarboxylic anhydride by microwave reaction, using cis-5-norbornene-inner-2,3-dicarboxylic anhydride as raw material, Specific steps are as follows:
[0036] (1) In a 1L reaction flask, stir 200g of cis-5-norbornene-endo-2,3-dicarboxylic acid anhydride and 800mL of butyl acetate evenly, put it in a microwave reaction kettle, heat up to 220°C, and The microwave reaction was carried out for 6 minutes under the microwave with a frequency of 10-100 GHz;
[0037] (2) After the reaction is complete, cool the reactor in step (1) to 100°C, place it in an oil bath and stir for 30 minutes to crystallize, cool to room temperature, filter, and dry to obtain the product cis-5-norbornene-exo Type-2,3-dicarboxylic acid anhydride 145.2g; yield: 72.6%; purity: 98.2%; oxide impurity content: 0.06%.
Embodiment 3
[0039] A method for preparing high-purity cis-5-norbornene-exo-2,3-dicarboxylic anhydride by microwave reaction, using cis-5-norbornene-inner-2,3-dicarboxylic anhydride as raw material, Specific steps are as follows:
[0040] (1) In a 1L reaction flask, stir 200g of cis-5-norbornene-endo-2,3-dicarboxylic acid anhydride and 600mL of toluene evenly, put it into a microwave reaction kettle, heat up to 200°C, at a frequency of Microwave reaction under 100-200GHz microwave for 8 minutes;
[0041] (2) After the reaction is completed, cool the reactor in step (1) to 110°C, place it in an oil bath and stir for 30 minutes to crystallize, cool to room temperature, filter, and dry to obtain the product cis-5-norbornene-exo Type-2,3-dicarboxylic acid anhydride 160.2g; yield: 80.1%; purity: 98.2%; oxide impurity content: 0.06%.
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