Diester-substituted methyl salicylate analogue and preparation method and application thereof
The technology of a drug and an alkyl group is applied to the methyl salicylate analog substituted by the diester group and its preparation, and the application fields in the control of aphids and the attraction of natural enemies can solve the problems of short shelf life, limited sources of volatiles and irregular structure. stability and other issues, to achieve the effects of low cost, simple and easy preparation method, and diverse functions
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Embodiment 1
[0056] Example 1, Preparation of 1-(E)-3,7-dimethyl-2,6-octadiene-2-(acetoxy)-3-methoxybenzoate (A-01)
[0057] In a 100 mL three-necked flask, 2.18 g of 3-methoxysalicylic acid, 3.22 g of DCC (dicyclohexylcarbodiimide) and 1.74 g of DMAP (4-dimethylaminopyridine) were added. Dissolve in 40 mL of tetrahydrofuran, add 2.00 g of geraniol dropwise, and react at 20°C for 3 h. Extract with water three times, obtain organic phase, remove solvent under reduced pressure, silica gel column chromatography (eluent is sherwood oil: ethyl acetate=V 1 :V 2 =50:1), a yellow liquid was obtained, and the product was 1-(E)-3,7-dimethyl-2,6-octadiene-2-hydroxyl-3-methoxybenzoate, the yield 53.8%.
[0058] In a 50mL three-necked flask, add 2g 1-(E)-3,7-dimethyl-2,6-octadiene-2-hydroxyl-3-methoxybenzoate (6.6mmol), then Add 30ml of dichloromethane to dissolve and stir well. Add 1.34g triethylamine (13.2mmol) afterwards as acid-binding agent, ice-bath cooling. Dissolve 1.05g of acetyl chlorid...
Embodiment 2
[0059] Example 2, 1-(E)-3,7-dimethyl-2,6-octadiene-2-(propionyloxy)-3-methoxybenzoate (A-02) preparation
[0060] In a 100 mL three-necked flask, 2.18 g of 3-methoxysalicylic acid, 3.22 g of DCC (dicyclohexylcarbodiimide) and 1.74 g of DMAP (4-dimethylaminopyridine) were added. Dissolve in 40 mL of tetrahydrofuran, add 2.00 g of geraniol dropwise, and react at 20°C for 3 h. Extract with water three times, obtain organic phase, remove solvent under reduced pressure, silica gel column chromatography (eluent is sherwood oil: ethyl acetate=V 1 :V 2 =50:1), a yellow liquid was obtained, and the product was 1-(E)-3,7-dimethyl-2,6-octadiene-2-hydroxyl-3-methoxybenzoate, the yield 53.8%.
[0061] In a 50mL three-necked flask, add 2g 1-(E)-3,7-dimethyl-2,6-octadiene-2-hydroxyl-3-methoxybenzoate (6.6mmol), then Add 30ml of tetrahydrofuran to dissolve and stir evenly. Then add 0.782g pyridine (9.9mmol) as an acid-binding agent, and cool down in an ice bath. Dissolve 1.22g of propi...
Embodiment 3
[0062] Example 3, 1-(E)-3,7-dimethyl-2,6-octadiene-2-(butyryloxy)-3-methoxybenzoate (A-03) preparation
[0063] In a 100 mL three-necked flask, 2.18 g of 3-methoxysalicylic acid, 3.22 g of DCC (dicyclohexylcarbodiimide) and 1.74 g of DMAP (4-dimethylaminopyridine) were added. Dissolve in 40 mL of tetrahydrofuran, add 2.00 g of geraniol dropwise, and react at 20°C for 3 h. Extracted three times with water to obtain the organic phase, removed the solvent under reduced pressure, and separated by silica gel column chromatography (eluent: petroleum ether: ethyl acetate = V1: V2 = 50:1) to obtain a yellow liquid, the product was 1-(E )-3,7-dimethyl-2,6-octadiene-2-hydroxy-3-methoxybenzoate, yield 53.8%.
[0064] In a 50mL three-necked flask, add 2g 1-(E)-3,7-dimethyl-2,6-octadiene-2-hydroxyl-3-methoxybenzoate (6.6mmol), then Add 30ml of ethyl acetate to dissolve and stir well. Then add 0.58g of butyric acid (6.6mmol) and 30ml of ethyl acetate solution to dissolve evenly, stir, a...
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