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A kind of preparation method of 2,4,6-tris(p-tert-butyloxyphenoxy)pyrimidine
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A technology of tert-butyloxyphenoxy and tert-butyloxyphenol, applied in the field of preparation of 2,4,6-tripyrimidine, which can solve the problems of high reaction temperature, harsh reaction conditions, and low reaction conversion rate , to achieve the effect of low reaction temperature, easy access to raw materials, and reasonable selection
Active Publication Date: 2019-04-19
内蒙古佳瑞米精细化工有限公司
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Disadvantages: high reaction temperature, low reaction conversion rate, many by-products, large amount of waste liquid
[0006] 2) With 2,4,6-trihydroxypyrimidine and p-tert-butyloxyfluorobenzene as raw materials, the reaction is carried out under high temperature and high pressure conditions, and the reaction conditions are not easy to meet
Disadvantages: harsh reaction conditions, low conversion rate, high raw material price and not easy to obtain
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Embodiment 1
[0033] At -20°C, p-tert-butyloxyphenol (16.622g, 0.1mol) was added to the organic solvent chloroform (141.3ml), and then 18-crown-6 (0.264g, 0.001mol), Potassium carbonate (6.910g, 0.05mol); slowly raise the temperature of the reaction system by 10°C (3-5°C / min), and keep it warm for 10min; then add 4,6-dichloro-2-thiamphenicol pyrimidine (4.541g, 0.02 mol); the reaction was slowly heated to 40°C (3-5°C / min), and kept for 4 hours; filtered, and the filtrate was distilled off the solvent under normal pressure to obtain the product. The spectrum of the obtained product is as Figure 1-2 shown.
[0034] The yield of the obtained product was 96%, and the purity detected by gas chromatography was 99.0%. The melting point of the product is 70-72°C.
Embodiment 2
[0036] At 0°C, p-tert-butyloxyphenol (16.622g, 0.1mol) was added to the organic solvent dichloromethane (166.2ml), and then 15-crown-5 (0.264g, 0.01mol) was added thereto , sodium hydroxide (4.002g, 0.1mol); the reaction system was slowly heated up to 20°C (3-5°C / min), and kept for 60min; then 4,6-dichloro-2-thiamphenicol pyrimidine (7.491g , 0.033mol); the reaction was slowly heated to 40°C (3-5°C / min), and kept for 1h; filtered, and the filtrate was distilled off the solvent under normal pressure to obtain the product. The yield is 85%, and the purity detected by gas chromatography is 99.1%.
Embodiment 3
[0038] At -10°C, p-tert-butyloxyphenol (16.622g, 0.1mol) was added to the organic solvent tetrahydrofuran (83.1ml), and then 18-crown-6 (1.322g, 0.005mol), Sodium carbonate (7.421g, 0.07mol); the reaction system was slowly heated up to 20°C (3-5°C / min), and kept for 20min; then 4,6-dichloro-2-thiamphenicol pyrimidine (5.675g, mol); the reaction was slowly heated up to 30°C (3-5°C / min), and kept for 2h; filtered, and the filtrate was distilled off the solvent under normal pressure to obtain the product. The yield is 90%, and the purity detected by gas chromatography is 99.5%.
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Abstract
The invention discloses a preparation method for 2,4,-6-tris(p-tert-butyl oxyphenoxy) pyrimidine, and belongs to the technical field of organic synthesis. According to the preparation method, a 2,4,-6-tris(p-tert-butyl oxyphenoxy) pyrimidine product is synthesized by taking 4,6-dichloro-methylsulfonyl pyrimidine and p-tert-butylphenol as raw materials, wherein the reaction temperature of a reaction system is 10 to 40 DEG C; the reaction time is 10 to 60 minutes. The method disclosed by the invention has the advantages that a technical route is selected reasonably and conveniently, and is easy to operate; according to the method, the raw materials are easily obtained, the cost is low, and reaction conditions are easy to realize. The yield of the 2,4,-6-tris(p-tert-butyl oxyphenoxy) pyrimidine product prepared by the method is 85 to 96 percent, and the product purity is greater than 99.0 percent.
Description
technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of 2,4,6-tris(p-tert-butyloxyphenoxy)pyrimidine. Background technique [0002] 2,4,6-tris(p-tert-butyloxyphenoxy)pyrimidine is an important pesticide raw material, widely used in medicine, pesticide and other fields. A large number of studies have shown that these compounds have good biological activities, such as insecticidal, weed-killing, anti-virus and anti-cancer. There are many methods reported in its synthesis literature, mainly in the following two ways: [0003] 1) Using 2,4,6-trichloropyrimidine and p-tert-butyloxyphenol as raw materials, undergo alkalization and dehydration, and then carry out addition reaction to obtain the product. Disadvantages: high reaction temperature, low reaction conversion rate, many by-products, and large amount of waste liquid. [0004] The reaction equation is as follows: [0005] [0006] 2...
Claims
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