Electric warming mosquito incense liquor and preparing method thereof
A technology of electric heating mosquito-repellent incense liquid and effective ingredients, which is applied in botany equipment and methods, chemicals for biological control, insecticides, etc. It can solve the problems of affecting the use effect and serious mosquito resistance, and reduce the use of insecticides. Quantity, avoid drug resistance, improve the effect of batch
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[0033] The present invention also provides a kind of synthetic method of limonoid, which comprises:
[0034] In the first step, chromium trioxide (11 g, 110 mmol) was slowly added to acetic anhydride (100 mL) at 0° C., and the reaction was stirred until orange, and the raw material Obacunone (45 g, 99.1 mmol) was added, And the temperature was raised to 60° C. and continued to stir for 3 hours. TLC (PE: EA = 2: 1) monitored the reaction end point. After the reaction was complete, the reaction solution was concentrated, and the concentrated solution was separated by ethyl acetate (200 mL) and water (200 mL). The organic phase was dried and concentrated with magnesium sulfate, and the crude product of the gained intermediate 2 was directly used in the next step reaction;
[0035]The second step; Intermediate 2 (46.0 g, 98.2 mmol) was dissolved in tetrahydrofuran (200 mL) and methanol (20 mL), and sodium borohydride (6.0 g, 150 mmol) was slowly added at 0°C to keep the internal t...
Embodiment 1
[0044] The preparation of embodiment 1 limonin
[0045] Slowly add chromium trioxide (11 g, 110 mmol) to acetic anhydride (100 mL) at 0°C, stir the reaction until orange, add raw material Obacunone (45 g, 99.1 mmol), and heat up to 60 Continue to stir at ℃ for 3 hours, TLC (PE:EA=2:1) to monitor the reaction end point, after the reaction is complete, the reaction solution is concentrated, the concentrated solution is separated by ethyl acetate (200 mL) and water (200 mL), and the organic phase is washed with sulfuric acid Magnesium was dried and concentrated, and intermediate 2 (46.0 g, 98.2 mmol) was dissolved in tetrahydrofuran (200 mL) and methanol (20 mL), and sodium borohydride (6.0 g, 150 mmol) was slowly added at 0°C to maintain the internal temperature of the reaction Not higher than 20°C, after the addition is complete, the reaction is stirred at 0°C for 1 hour, TLC (PE:EA=1:1) shows that the reaction is complete, the reaction solution is concentrated, and the conce...
Embodiment 2
[0048] Example 2 Electric Mosquito Repellent Liquid 1
[0049] Put 2 g of limonin, 0.3 g of d-allethrin, 0.06 g of triphenyl phosphate, and 0.6 g of antioxidant 2,6-di-tert-butyl-p-cresol (BHT) into a reaction vessel, and add water 400ml of solvent, heated to 50°C and stirred until completely dissolved, cooled to room temperature, then added ethanol solvent to 1L, and continued to stir for 1 hour to obtain electric heating mosquito repellent liquid 1.
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