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ChemicalBook CAS DataBase List N,N'-bis(2-methylphenyl)benzene-1,4-diamine

N,N'-bis(2-methylphenyl)benzene-1,4-diamine synthesis

6synthesis methods
-

Yield:15017-02-4 120 g

Reaction Conditions:

with 5%-palladium/activated carbon in water;N,N-dimethyl-formamide;benzene at 120; for 4 h;

Steps:

5 Example 5

To a four-necked flask equipped with a thermometer, a trap, and a condenser, 69 g (0.5 mol) of p-nitroaniline,123.2g (1.1mol) o-methylcyclohexanone, 17g catalyst Pd / C (content 5%, water content 60%),120mL of dimethylformamide and 20mL of benzene, heated to 120 ° C and refluxed, and continuously removed the water separated by the condensate;After 4 hours of holding temperature reaction, the condensate will not be water-separated, cool down, and filter the catalyst;The filtrate was distilled under reduced pressure, and benzene, dimethylformamide and a small excess of raw materials were distilled off.Get residue 120g,The sampling GC area normalization method determined that the content of bis (o-methylphenyl) -p-phenylenediamine was 96%.

References:

CN110734380,2020,A Location in patent:Paragraph 0077-0078