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10259-20-8

1-diphenylphosphoryloxy-4-nitro-benzene synthesis

4synthesis methods
-

Yield:10259-20-8 92%

Reaction Conditions:

with trifluoromethylsulfonic anhydride in dimethyl sulfoxide;acetonitrile at 90; for 12 h;Inert atmosphere;

Steps:

55

Take 4-nitrophenol (139mg, 1.0mmol) and diphenylphosphorus oxide (40.4mg, 0.2mmol) into a 10mL reaction tube, use a double-row tube to replace the air in the reaction tube with nitrogen, replace it three times, and then Trifluoromethanesulfonic anhydride (169 mg, 0.6 mmol), dimethyl sulfoxide (15.6 mg, 0.4 mmol) and 2.0 mL of acetonitrile were added, and the reaction was carried out at 90° C. for 12 hours. After the reaction, the organic phase was concentrated, and the mixture of petroleum ether and ethyl acetate with a volume ratio of 3:1 was used as the eluent, and the product 4-nitrophenyl diphenyl phosphate was obtained by column chromatography with a yield of 92 %.

References:

CN111606945,2020,A Location in patent:Paragraph 0317-0321