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ChemicalBook CAS DataBase List N,N-Dimethyl-1,4-phenylenediamine

N,N-Dimethyl-1,4-phenylenediamine synthesis

15synthesis methods
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Yield:99-98-9 95%

Reaction Conditions:

with 10% Pd/C;hydrogen in ethanol at 20; for 24 h;

Steps:

1.3 1-3. Synthesis of N1,N1-dimethyl-1,4-phenylenediamine (Compound 3)

10% Pd/c was put in a well-dried 2-neck flask equipped with a magnetic stirrer. The flask was purged with nitrogen to ensure nitrogen atmosphere inside the flask. N1,N1-dimethyl-1,4-nitroaniline was dissolved in ethanol absolute, and the flask was purged with hydrogen. The flask was sufficiently purged with hydrogen until the air inside the flask was replaced by hydrogen, followed by stirring at room temperature for 24 hours. 24 hours later, Pd/c used as a catalyst was filtered and separated from the product by using Cellite, followed by washing with ethanol. Water was added to a resulting brown solution and extracted with EtOAc. An extracted organic solution was washed with water and brine again. Thereafter, MgSO4 was added to the organic layer, followed by filtration. A filtrate was concentrated. A product had a brown solid phase (0.7 g, yield: 95%).

References:

US2019/92717,2019,A1 Location in patent:Paragraph 0057; 0066-0067

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