Synthesis method of dinotefuran
A synthesis method and dinotefuran technology are applied in many planting fields, can solve problems such as inconvenience, strong irritation, strong corrosion, etc., and achieve the effects of high yield, easy availability of raw materials and mild reaction conditions
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Embodiment 1
[0025] The present invention proposes a kind of synthetic method of dinotefuran, comprises the steps:
[0026] Use 3-formyl tetrahydrofuran as raw material to condense and reduce with 1,5-dimethyl-2-(nitroimino)-hexahydro-1,3,5-triazine, and then hydrolyze to obtain dinotefuran.
[0027] 3-formyl tetrahydrofuran synthetic steps are:
[0028] A, take furan as raw material, in the presence of catalyst TS-1, generate 1,4-butenedialdehyde with hydrogen peroxide oxidation;
[0029] B. Under weakly alkaline conditions, react with nitromethane to generate 2-nitromethyl-1,4-butanedialdehyde;
[0030] C. Dissolving 2-nitromethyl-1,4-butanedialdehyde in methanol, and reducing it with sodium borohydride at room temperature to generate 2-nitromethyl-1,4-butanediol;
[0031] D, 2-nitromethyl-1,4-butanediol is dehydrated and cyclized under the action of a strong acid catalyst to generate 3-nitromethyltetrahydrofuran;
[0032] E, 3-nitromethyl tetrahydrofuran is first oxidized with ozone ...
Embodiment 2
[0037] The preparation method of the catalyst TS-1 of furan oxidation ring-opening synthesis 1,4-butenedialdehyde, concrete steps are as follows:
[0038] According to U.S. Patent 4,410,501, 455 grams of tetraethyl silicate are placed in a single-necked flask equipped with a stirrer and kept in a carbon dioxide-free state, add 15 grams of titanium tetraethoxide (IV), and then gradually add 800 grams of 25% by weight Tetrapropylammonium hydroxide solution (without inorganic base). The mixture was stirred for about 1 hour, then heating was started carefully to accelerate the hydrolysis and evaporate the ethanol released. After about 5 hours at 80-90°C, the alcohol had evaporated completely. Increase the volume to 1.5 L with distilled water and transfer the milky homogeneous solution to an autoclave equipped with a stirrer. The mixture was heated to 175° C. and kept stirring at this temperature for 10 days under its own pressure. The autoclave was then cooled, the reaction mix...
Embodiment 3
[0040] 1, the synthesis of 4-butenedialdehyde, concrete steps are as follows:
[0041] Add 300 ml of acetonitrile, 21.0 g of furan (0.30 mol), silicon-titanium catalyst TS-1 (3 g) and hydrogen peroxide (35%, 0.36 mmol) into a 1000 ml one-necked flask. The mixture was stirred at room temperature for 2 hours, at which time the peroxide disappeared (detected with saturated aqueous potassium iodide). 200 ml of water was added to the reactant, the aqueous layer was extracted three times with dichloromethane, the organic layers were combined, dried over magnesium sulfate, filtered, and concentrated to obtain the product, 1H NMR (300MHz, DMSO-d6) δ9.60 (s, 2H), 7.32(s,2H).
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