3-氟-2,6-二氟苯腈

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In the same manner as in the process of the reduction step of Example 1, the reaction was carried out at 40° C. for 2.5 hours by using 10 g of 3-chloro-2,6-difluorobenzonitrile, 60 g of water, 0.25 g of palladium-carbon catalyst and 3 g of sodium hydroxide, and refinement was carried out to obtain 5.63 g of 2,6-difluorobenzonitrile.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: For example, when 3-chloro-2,6-difluorobenzonitrile is dissolved in methanol and reacted with hydrogen gas in the presence of palladium-carbon catalyst and triethylamine under the hydrogen pressure of 5 kg/cm2, the DFBN is obtainable. The DFBN is then heated and dissolved at 70° C. and dropwise added to 90% sulfuric acid, and the reaction is performed at 70° to 80° C. to obtain a 2,6-difluorobenzamide. The product is then dissolved in 1,2-dichloroethane and an oxyalyl chloride is dropwise added to the solution at 20° to 40° C., and the reaction is performed under reflux to obtain 2,6-difluorobenzoyl isocyanate. A dioxane solution of 3,5-dichloro-4-(3-chloro-5-trifluoromethyl-2-pyridyloxy) aniline is dropwise added to a dioxane solution of the isocyanate at 40° to 50° C. and the reaction was performed to obtain N-(2,6-difluorobenzoyl)-N'-[3,5-dichloro-4-(3-chloro-5-trifluoromethyl-2-pyridyloxy)phenyl]urea having a melting point of 203° to 205° C. This derivative is effective to combat a various kinds of undesirable insects, as disclosed in the Japanese Unexamined Patent Publication 125677/1979, U.S. Pat. Nos. 4,173,637, 4,173,638 and 4,310,530. The DFBN is then heated dissolved at 70° C. is performed at 70° to 80° C.

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Aqueous ammonia (d 0.880, 2 ml) was added to a solution of 3-chloro-2,6-difluorobenzonitrile (1.93 g, 11.1 mmol) in acetonitrile (10 ml), and the mixture heated to 60° C. for 16 h. The resulting brown solution was evaporated and purified by flash chromatography eluting with 5% ethyl acetate/hexane, increasing the gradient to 20% ethyl acetate/hexane, to furnish a white solid (410 mg), MS (+EI) 173/171 (M+); 1H NMR (CDCl3) 7.39 (1H, dd, J5.7, 9.0 Hz), 6.46 (1H, t, J8.7 Hz), 4.95 (2H, br. s). The resulting brown solution was evaporated purified by flash chromatography eluting with 5% ethyl acetate/hexane increasing the gradient to 20% ethyl acetate/hexane