Method for synthesizing geranylacetone with Carroll reaction
A kind of geranyl acetone, reaction technology, applied in the synthesis of spices, synthetic geranyl acetone field by Carroll reaction, can solve problems such as high production cost, difficult to recover, unstable catalyst, achieve high reaction yield, The effect of avoiding environmental pollution
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Embodiment 1
[0019] Add 500g of linalool and 20g of aluminum oxide to a 2000ml reaction kettle equipped with mechanical stirring, turn on the mechanical stirring, raise the temperature to 150°C, start to add 414g of methyl acetoacetate dropwise, add dropwise for 3.5h, and steam while adding The methanol generated by the reaction is directly connected to the gas storage tank to collect the generated carbon dioxide gas. After dripping and keeping warm for 5 hours, the reaction is completed. After the reaction is completed, 20g of the catalyst is filtered out, and the fore distillation is collected (top temperature 40-70°C, Methyl acetoacetate with a GC content of 57%, linalool with a GC content of about 34%) enters the next batch of feed, collects fractions with a top temperature of 105°C-110°C, and obtains 488.8g of geranylacetone with a content of 99%. Yield: 77.6%.
Embodiment 2
[0021] Add 500g of linalool and 20g of aluminum oxide (from the aluminum oxide recovered in Example 1) to a 2000ml reactor equipped with mechanical stirring, turn on the mechanical stirring, raise the temperature to 170°C, and start adding 414g of acetoacetic acid dropwise Methyl ester, add dropwise for 3.5 hours, distill the methanol produced by the reaction while adding dropwise, the reaction is directly connected to the gas storage tank to collect the generated carbon dioxide gas, the reaction is completed after dripping and keeping warm for 3 hours, and the catalyst is filtered out after the reaction. 19.8g, the catalyst Can be recycled, vacuum distillation, collect fore distillation (top temperature 40-70°C, methyl acetoacetate GC content 58%, linalool GC content 26%) into the next batch of feeding, collection top temperature 105°C-110°C The distillate obtains the geranylacetone of 537.28g content 99%. Yield: 85.3%.
Embodiment 3
[0023] Add 500g of linalool and 19.80g of aluminum oxide (from the aluminum oxide recovered in Example 2) to a 2000ml reactor equipped with mechanical stirring, turn on the mechanical stirring, raise the temperature to 180°C, and start adding 414g of acetyl Add methyl acetate dropwise for 3.5 hours, and distill the methanol produced by the reaction while adding dropwise. The reaction is directly connected to the gas storage tank to collect the generated carbon dioxide gas. After dripping and keeping warm for 2 hours, the reaction ends. After the reaction, 19.70 g of the catalyst is filtered out. Catalyst can be recycled, vacuum distillation, collected fore distillation (top temperature 40-70 ℃, methyl acetoacetate GC content about 60%, linalool GC content about 30%) into the next batch of feeding, to obtain 524.68g content 99 % of geranylacetone. Yield: 83.3%.
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