Cyanoacrylate compounds containing fluoro pyridine-methylamino group and their bioactivity
A fluoropicolinyl amino, cyanoacrylate technology, applied in the directions of biocides, plant growth regulators, chemicals used for biological control, etc., can solve the problem of no specific records, no specific records of compounds Herbicidal activity and other issues, to achieve the effects of excellent selectivity, increased selectivity, and safe growth
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Embodiment 1
[0039] Embodiment 1: 2-cyano-3, the synthesis of ethyl 3-dimethylthioacrylate
[0040] In a 250ml three-necked flask, add 17.1 grams of finely ground potassium hydroxide powder (0.25mol), and 100ml of dioxane. Cool to 0°C, add 14.1 g of ethyl cyanoacetate (0.125 mol), 9.5 g of carbon disulfide (0.125 mol), and 30 ml of dioxane solution dropwise under vigorous stirring, and add dropwise in about 2 hours. React at room temperature for 2-3 hours, stop the reaction, let it stand, and pour off the upper layer of dioxane to obtain a solid yellow solid. Continue to add 240ml of 95% ethanol and 40ml of water to the reaction flask. Add 34.65 g of dimethyl sulfate (0.275 mol) dropwise at room temperature under stirring, and complete the dropwise addition in 2-4 hours, continue to react at room temperature for about 5 hours, add 1500 ml of water to the system, stir, and precipitate a yellow solid product.
Embodiment 2
[0041] Example 2: Synthesis of 2-cyano-3,3-dimethylthioacrylic acid substituted phenoxyethyl ester
[0042] 0.0634mol potassium hydroxide and 0.0317mol 2-cyanophenoxyethyl ester (1) were added to 20mL of acetonitrile, and 0.0317mol carbon disulfide was added dropwise after 0.5h. After 3 h, 0.0665 mol of dimethyl sulfate was added dropwise under ice-cooling, and the mixture was naturally raised to room temperature, and stirred overnight. Suction filtration, spin dry, recrystallization.
Embodiment 3
[0043] Embodiment 3.2-cyano-3, the synthesis of ethoxyethyl 3-dimethylthioacrylate
[0044] In a 100ml three-necked flask, add 2.74 grams of finely ground potassium hydroxide powder (0.04mol), and 12ml of anhydrous acetonitrile, and after cooling to 5°C, add 2.86 grams of ethoxyethyl cyanoacetate (0.02mol) dropwise, 1.5 The mixed solution of carbon disulfide (0.02mol) and 5ml of anhydrous acetonitrile was dropped in about 30 minutes. Stir at room temperature for 4 hours. Cool to 0°C, add 5.04 grams of dimethyl sulfate (0.04mol) dropwise, complete the dropwise addition in 2 hours, continue to react at room temperature for about 5 hours, add 50ml of water to the system, and separate the generated red oil, namely for the product.
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