Method for preparing isoprothiolane
A technology of Daobunling and alkaline aqueous solution, which is applied in the field of pesticides, can solve the problems of high cost, low synthesis yield of Daobunling, and long process time, and achieve the effects of reducing production costs, shortening process time, and reducing consumption
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[0012] The invention provides a preparation method of rice blast spirit, which comprises firstly mixing diisopropyl malonate, carbon disulfide and alkaline aqueous solution uniformly, then adding dichloroethane and a catalyst, cooling and purifying after reaction to obtain the rice blast Spirit; Wherein, the catalyzer is an alkylpyridine chloride.
[0013] Preparation method provided by the invention, with diisopropyl malonate (C 9 h 16 o 4 ), carbon disulfide (CS 2 ), alkaline aqueous solution and dichloroethane (ClCH 2 CH 2 Cl) as a raw material, and the rice blastin was synthesized by a phase transfer catalysis method. Wherein alkaline aqueous solution is example with sodium hydroxide aqueous solution, and described reaction mechanism is as follows:
[0014]
[0015] As the common knowledge of those skilled in the art, the synthesis yield of the rice blastin is only about 60% under the condition of no catalyst. Therefore, by using various catalysts in the prior ar...
Embodiment 1
[0026] Add 1 mol of diisopropyl malonate and 1.1 mol of carbon disulfide into a reaction kettle equipped with electric stirring, thermometer, reflux condenser, and dropping tank, start stirring, and add 4.5 mol of sodium hydroxide aqueous solution (hydrogen) dropwise at 30°C The molar ratio of sodium oxide to water is 2:1); after dropping, keep the temperature in the reactor constant and continue to stir for 30 minutes. Then, 2 mol of dichloroethane was added from the dropping tank, and then 10 g of catalyst-1-dodecylpyridine chloride was added, and the mixture was refluxed at 70° C. for 1 h. After the reaction was completed, the layers were allowed to stand still. The lower organic phase was removed to remove dichloroethane. After cooling, the product is crystallized and pulverized to obtain a light yellow sample of rice blastin, which is denoted as S1. S1 was weighed and calculated to obtain a purity of 95.8% and a synthesis yield of 91.5%.
Embodiment 2
[0028] Add 1 mol of diisopropyl malonate and 1.1 mol of carbon disulfide into a reaction kettle equipped with electric stirring, thermometer, reflux condenser, and dropping tank, start stirring, and add 4.5 mol of potassium hydroxide aqueous solution (hydrogen The molar ratio of potassium oxide to water is 2:1); after dropping, keep the temperature in the reactor constant and continue to stir for 35 minutes. Then, 2 mol of dichloroethane was added from the dropping tank, and 15 g of catalyst 1-butylpyridine chloride was added, and reflux reaction was carried out at 75°C for 1.5 h. After the reaction was completed, the layers were allowed to stand still. The lower organic phase was removed to remove dichloroethane. After cooling, the product crystallizes and then pulverizes to obtain a pale yellow rice blastin sample, which is denoted as S2. S2 was weighed and calculated to obtain a purity of 96.2% and a synthetic yield of 92.1%.
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