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3AMINO2NITROBIPHENYL synthesis

3synthesis methods
-

Yield:96187-18-7 71%

Reaction Conditions:

with tetrakis-(triphenylphosphine)-palladium;anhydrous sodium carbonate in 1,4-dioxane;lithium hydroxide monohydrate at 85; for 8 h;Inert atmosphere;

Steps:

4 2'-nitro-[1,1'-biphenyl]-3-amine (22)

To a three-necked flask containing 0.33g (2.0mmol) of compound 20 was added 0.38g (2.2mmol) of compound 21, 0.42g (4.0mmol) Na2CO3, 0.12g (0.05mmol) Pd(PPh3) 4, 30mL 1,4- dioxane/H2O(4/1,v/v). The reaction mixture was replaced with N2 for 15 minutes, and then the system was placed at 85°C for 8 hours. After the reaction was completed, cooled to room temperature, filtered through Celite, added 200 mL of water to the filtrate, and extracted with 50 mL of ethyl acetate (×3). The organic phase was washed with saturated brine, dried over Na2SO4, and concentrated in vacuo. The crude product was purified by Flash column to obtain 0.31 g. Yield: 71%. Yellow solid 22.

References:

CN111333639,2020,A Location in patent:Paragraph 0098-0101