Method for preparing 11-methoxyl-3,7,11-trimethyl-2,4-dodecadienoate
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A technology of isopropyl carbadienoate and ammonium carbadienoate, which is applied in the field of preparation of insect growth regulators, can solve the problems of high cis-ester content, affecting product performance, unqualified and the like, avoiding hydrolysis, The effect of high pass rate
Inactive Publication Date: 2009-03-25
常州胜杰生命科技股份有限公司
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Since ammonia gas will be generated during the reaction, the cis-ester content of the final product will be higher. Since the cis-ester has no effect on insects, it is an impurity, which will affect the performance of the product. Usually, products with higher cis-ester unqualified
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Embodiment 1
[0008] The preparation method steps of 11-methoxy-3,7,11-trimethyl-2,4-dodecadienoic acid isopropyl ester of the present embodiment are as follows:
[0009] ① Under a nitrogen atmosphere and stirring, put 54kg of n-hexane and 90kg of 11-methoxyl-3,7,11-trimethyl-2,4-dodecane into a reactor with a reflux condenser successively Dienoic acid ammonium salt (315.8 mol) and 103 kg of tetraisopropyl titanate (362.7 mol). Among them, n-hexane and tetraisopropyl titanate are industrial-grade raw materials.
[0010] ② Turn on the vacuum and keep the vacuum for 5 minutes after reaching 0.05Mpa.
[0011] ③Raise the temperature slowly to 105°C within 25-30 minutes, and maintain at this temperature for 5 minutes to remove ammonia gas.
[0012] ④Raise the temperature to 150°C within 8 to 12 minutes, turn off the vacuum, and keep the temperature at this temperature for 1 hour to complete the reaction.
[0013] 5. the reaction product is rapidly reduced to 10 DEG C, and 53kg of normal hexan...
Embodiment 2～ Embodiment 5
[0015] The preparation method of each embodiment is basically the same as that of Example 1, and the differences are shown in Table 1.
[0016]
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Abstract
The invention discloses a method for preparing 11-anisyl-3, 7, 11-trimethyl-2, 4-dodecadienoic acid isopropyl ester, which comprises the steps that: 1) normal hexane, 11-anisyl-3, 7, 11-trimethyl-2, 4-dodecadienoic acid ammonium salt and tetraisopropyl titanium ester are sequentially added into a reaction kettle at the nitrogen atmosphere when stirring; 2) the vacuum is started to lead the vacuum degree to achieve 0.04 to 0.06MPa and be kept for 4 to 6min; 3) within 25 to 30min, the temperature is slowly raised to 100 to 105 DEG C and kept for 4 to 6min, and the ammonia gas is removed; 4) within 8 to 12min, the temperature is raised to 145 to 150 DEG C, the vacuum is closed, and the reaction is complete at the temperature of 145 to 150 DEG C; and 5) the temperature of the reaction products is quickly reduced to 8 to 12 DEG C, the normal hexane is added, and then the mixture is poured into sulphuric acid, thus obtaining the final products after washing and solvent removing. The products prepared by the method have lower cis-ester content, and are all qualified.
Description
technical field [0001] The invention relates to a preparation method of an insect growth regulator, in particular to a preparation method of 11-methoxy-3,7,11-trimethyl-2,4-dodecadienoic acid isopropyl ester. Background technique [0002] Canadian patent document CA1054628A1 discloses a method for synthesizing fatty acid esters with tetraalkyl titanate and fatty acid or its ammonium salt. Wherein the molar ratio of tetraalkyl titanate to fatty acid or its ammonium salt is 0.75:1˜1.5:1. The reaction temperature is 110-200°C, and the reaction time is 1-2 hours. Wherein the fatty acid is 11-methoxy-3,7,11-trimethyl-2,4-dodecadienoic acid (11-methoxy-3,7,11-trimethyl-2,4-dodecadienoic acid), 11-ethoxy-3,7,11-trimethyl-2,4-dodecadienoic acid (11-ethoxy-3,7,11-trimethyl-2,4-dodecadienoic acid) or 3,7 , 11-trimethyl-2,4-dodecadienoic acid (3,7,11-trimethyl-2,4-dodecadienoic acid), and mainly (2E, 4E) isomers. The fatty acid ester generated is 11-methoxy-3,7,11-trimethyl-2,4-dod...
Claims
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