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ChemicalBook CAS DataBase List Benzenamine,N,N-bis(2-chloroethyl)-4-nitro-
55743-71-0

Benzenamine,N,N-bis(2-chloroethyl)-4-nitro- synthesis

5synthesis methods
-

Yield:55743-71-0 95%

Reaction Conditions:

with thionyl chloride;triethylamine in dichloromethane; for 3 h;Reflux;Time;

Steps:

1.2 synthesis of N,N-bis(2-chloroethyl)-4-nitroaniline

2.70 g (0.012 mol) of yellow needle-like crystals, N, N-bis (2-hydroxyethyl) -4-nitroaniline,N-bis (2-hydroxyethyl) -4-nitroaniline,Was dissolved in 60. 0 mL of dry dichloromethane, and then 1. ml of triethylamine was added to the reaction flask. 1.3 ml (0.018 mol) of thionyl chloride was dissolved in 20.0 mL of dichloromethane,The solution was added dropwise to the reaction flask at room temperature with stirring for 1 h. After completion of the dropwise addition, the temperature was raised to 40 ° C and the reaction was stirred for 2 hours under reflux. After completion of the reaction, the mixture was allowed to stand for cooling and diluted with 30.0 mL of dry methylene chloride. The organic layers were washed with 20.0 mL of saturated sodium bicarbonate solution and the combined organic layers were dried over anhydrous sodium sulfate. The solvent was removed by distillation under reduced pressure to give N , Crude N-bis (2-chloroethyl) -4-nitroaniline. The crude product was recrystallized from anhydrous ethanol to give 2.99 g of yellow needle-like crystals N, N-bis (2-chloroethyl) -4-nitroaniline in a yield of 95.0%

References:

CN106631876,2017,A Location in patent:Paragraph 0045; 0049-0052