Method for preparing sex pheromone of carpocapsa pomonella
A codling moth and pheromone technology, which is applied in the field of preparation of codling moth sex pheromone, can solve the problems of low unfavorable industrial production, long synthesis route, cumbersome operation steps, etc., and achieve easy large-scale industrial production and product structure. Good shape and simple operation
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Embodiment 1
[0028] Under the protection of nitrogen, 200g (0.425mol) 8-hydroxyoctyltriphenylphosphine bromide was dissolved in 2L methyl tert-butyl ether solution, and 108.93g (1.7mol) n-butyllithium was dissolved at -78℃. Add 2.6L of n-hexane solution to the above system, stir until the color of the system is dark red; add 29.8g (0.425mol) 2E-crotonaldehyde in 400mL n-hexane solution, react until the color of the system becomes lighter, add 28.92g( 0.213mol) potassium dihydrogen phosphate solid inactivates the reaction. Add 3L of water to the reaction mixture, separate the organic layer, continue to extract the water layer with n-hexane, and use anhydrous Na for the organic layer 2 SO 4 Drying, distillation under reduced pressure, GC and GC-MS analysis shows that the target product obtained by distillation under reduced pressure is E, E-8, 10-dodecadien-1-ol, weighing 65.87g, and subjected to GC external standard The quantitative method was 97%, and the yield was 83%.
Embodiment 2
[0030] Under the protection of nitrogen, dissolve 100g (0.213mol) of 8-hydroxyoctyltriphenylphosphine bromide in 1.2L of diethyl ether, maintain the temperature at -78℃, and add 37.7g (0.639mol) of butyllithium to 1.1L of n-hexane Add the alkane solution to the above system and stir until the color of the system is dark red; cool the reaction solution to below -70°C, add 14.9g (0.213mol) 2E-crotonaldehyde in 100mL n-hexane solution dropwise, and react until the system color changes Shallow, the reaction system was gradually heated to 20°C, and 14.46g (0.106mol) potassium dihydrogen phosphate solid was added to inactivate the reaction. Add 1.5L water to the reaction mixture, separate the organic layer, continue to extract the water layer with n-hexane, and use anhydrous Na for the organic layer 2 SO 4 Drying, distillation under reduced pressure, GC and GC-MS analysis shows that the target product obtained by distillation under reduced pressure is E, E-8, 10-dodecadien-1-ol, with ...
Embodiment 3
[0032] Under the protection of nitrogen, dissolve 150g (0.319mol) of 8-hydroxyoctyltriphenylphosphine bromide in 1.8L methyl tert-butyl ether, maintain the temperature at -78℃, and add 102.23g (1.595mol) n-butyl Add 2.8L benzene solution of base lithium to the above system, stir until the color of the system is dark red; add 22.3g (0.319mol) 2E-crotonaldehyde in 300mL n-heptane solution, react until the color of the system becomes lighter, add 19.14 g (0.159mol) potassium dihydrogen phosphate solid inactivates the reaction. Add 500 mL of water to the reaction mixture, separate the organic layer, continue to extract the aqueous layer with n-heptane, and use anhydrous Na for the organic layer 2 SO 4 Drying, distillation under reduced pressure, GC and GC-MS analysis shows that the target product obtained by distillation under reduced pressure is E, E-8, 10-dodecadien-1-ol, and the weight is 53.3g. The quantitative method is 95%, and the yield is 87%.
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