Thioether kind bacteriocide
A technology of compound and general formula, applied in the field of agricultural fungicides
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example 1
[0070] The preparation of example 1 intermediate (V)
[0071]
[0072] Add 45 grams of phenol, 2.4 grams of formaldehyde, and 4.96 grams of ethanethiol to the reaction flask equipped with a stirrer and a condenser, and heat up to reflux. After reacting for 8 hours, the mixture was dephenolized by distillation and vacuum distillation to obtain 8.99 g of 2-ethylthiomethylphenol product with a content of 98% and a yield of 66.5%.
[0073] 1 HNMR: 1.22(3H, t), 2.42(2H, m), 3.81(2H, s), 6.84(1H, m), 7.89(1H, t), 7.08(1H, m), 7.19(1H, m) .
example 2
[0074] Example 2 Preparation of Compound 2
[0075]
[0076] Add 30 milliliters of N, N-dimethylformamide, 10.8 millimoles of anhydrous potassium carbonate, 1.76 grams (10.5 millimoles) of compound (V) and 2.85 grams (10 millimoles) in the reaction flask equipped with stirrer and condenser millimole) compound (VI), then heated to 60 ° C and stirred for 6 hours. The reaction solution was cooled and poured into 200 ml of water, extracted three times with ethyl acetate (3×150 ml), the extract was dried over anhydrous magnesium sulfate and concentrated to obtain a crude product. Column chromatography (developing solvent: ethyl acetate:petroleum ether=1:5) gave pure compound 2, weighing 3.01 g (yield 81%).
[0077] 1 HNMR: 1.22(3H,t), 2.49(2H,m), 3.70(3H,s), 3.81(2H,s), 3.83(3H,s), 5.02(2H,s), 6.78(1H,d) , 6.89 (1H, t), 7.17 (2H, m), 7.28 (3H, m), 7.61 (1H, m), 7.63 (1H, s).
example 3
[0078] Preparation of Example 3 Compound 6
[0079]
[0080] Add 30 milliliters of N,N-dimethylformamide and 0.53 grams (22.0 mmol) of sodium hydride washed with petroleum ether into a reaction flask equipped with a stirrer and a condenser, and add 3.36 grams of it under stirring at room temperature. (20.0 mmol) 20 milliliters of N, N-dimethylformamide solution of compound (V), there is gas evolution, and the dropwise addition is completed in 20 minutes, and then stirred for another 30 minutes without gas emission. Add 5.72 g (20 mmol) compound (VI) / 35 ml N,N-dimethylformamide solution, react at room temperature for 3 h, stop stirring. The reaction solution was poured into 400 ml of water, extracted three times with ethyl acetate (3×250 ml), the extract was dried over anhydrous magnesium sulfate, and then concentrated to obtain a crude product. Column chromatography (eluent: ethyl acetate:petroleum ether=1:5) yielded 5.97 g of pure compound 6 (yield 80%).
[0081] 1 HNMR...
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