N,N,N',N'-Tetrakis(4-aminophenyl)-1,4-benzenediamine synthesis

Yield:3283-07-6 99%

Reaction Conditions:

with ferric(III) chloride;iron(III) oxide;pyrographite;hydrazine in lithium hydroxide monohydrate;N-methylpyrrolidine N-oxide at 100 - 110; for 6 h;Product distribution / selectivity;

Steps:

4

Example 4: Production of Compound (III-l) 160 g of Compound (II-l), 1.07 g of iron (III) chloride 6-hydrate, 1.55 g of iron (III) oxide, 16.2 g of activated carbon, and 1400 ml of l-methyl-2-pyrrolidone were put into a three-neck flask, and heated with stirring up to an inner temperature of 100⁰C. 450 g of hydrazine monohydrate (aqueous 80% solution) was dropwise added thereto, taking 1 hour, then this was kept stirred under heat at an inner temperature of from 100 to 110⁰C for 5 hours, and thereafter cooled to room temperature. This was filtered to remove the activated carbon, then 800 ml of methanol and 1200 ml of water were continuously dropwise added thereto, and the resulting crystal was taken out through suction filtration to obtain 126.3 g of the intended Compound (III-l) (yield, 99%). Its mass spectrum gave M/e = 472.

References:

WO2007/73000,2007,A1 Location in patent:Page/Page column 33