Carbamate sterilization compound containing vinyl oxime ether
A carbamate, vinyl oxime technology, applied in the direction of fungicides, biocides, chemicals for biological control, etc., can solve the problem that carbamate fungicidal active compounds are not reported in literature and so on
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Embodiment 1
[0031] Preparation of the compound N-methoxy-N-2-[1-(2-phenylvinyl) ethyleneiminooxymethyl] phenyl carbamate (compound 1)
[0032] To 20ml of toluene, add 0.64g (4mmol) of 1-(2-phenylvinyl)-acetaldoxime and 0.25g (5mmol) of 60% NaH, and add 1.37g( 5.0 mmol) N-(2-bromomethylphenyl)-N-methoxy-carbamic acid methyl ester in toluene. After dripping, react at this temperature for 10-15 minutes, and wash the reactant with water until it is neutral and anhydrous Na 2 SO 4 Dry and desolvate under reduced pressure to obtain crude product. The crude product was washed by column chromatography with a mixture of ethyl acetate and petroleum ether (1:3) to obtain 0.54 g of the target compound with a yield of 38.3%.
[0033] Target compound 1 H NMR(300MHZ, CDCl 3 ): 2.14 (s, 3H, CH3), 3.77, 3.79 (2s, 6H, 2OCH3), 5.25 (s, 2H, CH2O), 6.78 ~ 6.91 (q, 2H, CH = CH), 7.25 ~ 7.55 (m, 9H, Ar-H)
Embodiment 2
[0035] Preparation of N-methoxy-N-2-[1-(2-(3-chlorophenyl)-vinyl)ethyliminooxymethyl]phenylcarbamate (compound 3)
[0036] To 20ml dimethylformamide, add 0.92g (5mmol) of 1-(2-(3-chlorophenyl)vinyl)-acetaldoxime, 0.42g (3mmol) potassium carbonate, 1.37g (5mmol) N -(2-Bromomethylphenyl)-N-methoxy-carbamic acid methyl ester. Stir at 25~30℃ for 1 hour. After the reaction is complete, the reaction solution is poured into 100ml of water and extracted twice with ethyl acetate. The ethyl acetate layer is washed with water to neutrality, and then with anhydrous Na 2 SO 4 After drying and removing the solvent, a crude product is obtained. The crude product was washed by column chromatography with a mixture of ethyl acetate and petroleum ether (1:3) to obtain 1.16 g of the target compound with a yield of 60%.
[0037] Target compound 1 H NMR(300MHZ, CDCl 3 ): 2.12(s, 3H, CH3), 3.76, 3.79(2s, 6H, 2×OCH3), 5.25(s, 2H, CH2O), 6.79(s, 2H, CH=CH), 7.24~7.53(m, 8H, Ar-H)
Embodiment 3
[0039] Preparation of N-methoxy-N-2-[1-(2-(4-chlorophenyl)-vinyl) ethyleneiminooxymethyl] phenyl carbamate (compound 4)
[0040] To 20ml dimethylformamide, add 0.92g (5mmol) of 1-(2-(4-chlorophenyl)vinyl)-acetaldoxime, 0.42g (3mmol) potassium carbonate, 1.37g (5mmol) N-(2-Bromomethylphenyl)-N-methoxy-carbamic acid methyl ester.
[0041] Stir at 25-30°C for half an hour. After the reaction is complete, the reaction solution is poured into 100ml of water and extracted twice with ethyl acetate. The ethyl acetate layer is washed with water until it is neutral, and then with anhydrous Na 2 SO 4 After drying and removing the solvent, a crude product is obtained. The crude product was washed by column chromatography with a mixture of ethyl acetate and petroleum ether (1:3) to obtain 1.22 g of the target compound with a yield of 62%.
[0042] Target compound 1 H NMR(300MHZ, CDCl 3 ): 2.09(s, 3H, CH3), 3.75, 3.76(2s, 6H, 2×OCH3), 5.21(s, 2H, CH2O), 6.82, 6.88(d, 2H, CH=CH), 7.27~7.55( m, 8...
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