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With ammonium formate; zinc; In methanol; water; for 1.33333h;
To a solution of <strong>[3107-19-5]1,3-dichloro-2-fluoro-5-nitro-benzene</strong> (71.4 g, 340 mmol) in methanol (1.5 L) was added a solution of ammonium formate (180.2 g, 2.86 mol) in water (300 mL). Zinc dust (93.4 g, 1.43 mol) was then added in four equal portions over 20 min. The reaction was stirred for 1 h and then allowed to cool to room temperature. The reaction mixture was filtered through diatomaceous earth and the filtrate was concentrated in vacuo. Ethyl acetate (300 mL) and water (300 mL) were added and the mixture was again filtered through diatomaceous earth. The layers were separated, and the aqueous layer was further extracted with ethyl acetate (350 mL). The combined organics were washed with 500 mL of brine, dried over Na2SO4, filtered, and concentrated to afford 56.4 g of the title compound as a brown solid, mJz 180.2 [M+H]+. This material was used without any further purification.
With ammonium formate; zinc; In methanol; water; for 1.33333h;
To a solution of l,3-dichloro-2-fluoro-5-nitro-benzene (71.4 g, 340 mmol) in methanol (1.50 L) was added a solution of ammonium formate (180 g, 2.86 mol) in water (300 mL). Zinc dust (93.4 g, 1.43 mol) was then added in four equal portions over 20 min. The reaction was stirred for 1 h and then allowed to cool to room temperature. The reaction mixture was filtered through diatomaceous earth and the filtrate was concentrated in vacuo. Ethyl acetate (300 mL) and water (300 mL) were added and the mixture was again filtered through diatomaceous earth. The layers were separated, and the aqueous layer was further extracted with ethyl acetate (350 mL). The combined organics were washed with 500 mL of brine, dried over Na2SO4, filtered, and concentrated to afford 56.4 g of the title compound as a brown solid, tn/z 180.2 [M+H]+. This material was used without any further purification.
With ammonium formate;zinc; In methanol; water; at 20℃;
3,5-Dichloro-4-fluoro-phenylamine:To a solution of l,3-dichloro-2-fluoro-5-nitro-benzene (71.4 g, 340 mmol) in methanol (1.5 L) was added a solution of ammonium formate (180.2 g, 2.86 mol) in water (300 mL). Zinc dust (93.4 g, 1.43 mol) was then added in four equal portions over 20 min. The reaction was stirred for 1 h and then allowed to cool to room temperature. The reaction mixture was filtered through diatomaceous earth and the filtrate was concentrated in vacuo. Ethyl acetate (300 niL) and water (300 niL) were added and the mixture was again filtered through diatomaceous earth. The layers were separated, and the aqueous layer was further extracted with ethyl acetate (350 niL). The combined organics were washed with 500 mL of brine, dried over Na2SO4, filtered, and concentrated to afford 56.4 g of the title compound as a brown solid, m/z 180.2 [M+H]+. This material was used without any further purification.
With palladium on activated charcoal; hydrogen; N-Cyanoguanidine; In ethanol; at 55℃; for 1h;
The corn stover is pulverized and freeze-dried at -10 C.After being taken out, it is mixed with melamine sodium polyphosphate and ethanol and ground to ethanol for evaporation.Preparing a mixed powder; mixing and mixing the mixed powder and dicyandiamide in a muffle furnace,The calcination treatment is carried out at 750 C for 1 h to prepare a cocatalyst; wherein, corn stalk,The mass ratio of melamine sodium polyphosphate and dicyandiamide is 3:0.023:0.5; Adding <strong>[3107-19-5]3,5-dichloro-4-fluoronitrobenzene</strong>, water and dicyandiamide to the reactor, stirring and mixing, adding palladium/carbon catalyst,a cocatalyst, introducing nitrogen gas into the reactor for 5-10 minutes to displace the air in the reactor.Then, hydrogen gas was introduced to a pressure of 18 kg, and the reaction was carried out at 55 C for 1 hour, and after the reaction was completed, it was cooled to room temperature.Detecting the content of the target product in the product; wherein <strong>[3107-19-5]3,5-dichloro-4-fluoronitrobenzene</strong>, water, dicyandiamide,The mass ratio of the palladium/carbon catalyst was 3:2:0.0015:0.001; the mass ratio of the palladium/carbon catalyst to the cocatalyst was 1:0.3.
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