2,2'-[[3-acetamido-4-[(4-nitrophenyl)azo]phenyl]imino]diethyl diacetate synthesis

Yield:-

Reaction Conditions:

Stage #1: 4-nitro-aniline;3-(N,N-di(acetyloxyethyl)amino)-N-phenylacetamidewith 1-ethenyl-2-pyrrolidinone;nitrosylsulfuric acid;sulfuric acid at 0 - 5; for 2 h;Inert atmosphere;Large scale;
Stage #2: with ammonia at 65 - 70; pH=6 - 7; for 1 h;Large scale;pH-value;Reagent/catalyst;Temperature;

Steps:

2 Example 2

Diazo successively invested in 98% sulfuric acid tank 1000kg, 28% nitrosyl sulfuric acid 3150kg,Open freezing brine cooling with stirring, slowly put right nitroaniline 900kg, the following addition was completed, 5 , PaulTemperature to complete the reaction,spare;Coupling was added into the kettle bottom water 15000kg, added 25kgPeregal and 735kgN, N- diethyl acryloyloxyethyl - Inter-acetylaminoaniline, 2 hours after the beating,Digging ice cooling and then added to theHeavy nitrogen liquid, plus complete 0 ~ 5 incubated for 6 hours to detect the end after passing start adding ammonia solution (mass percentage concentration of 18%) adjusting the pH value to 6.0 to 7.0, and then heated up to 65 ~ 70 ,Stirred for an hour for the transfer dye transfer crystal grain backward filter press filtration, washed with water until neutral to give 74 red disperse dye cake, prepared after the mother liquor of ammonium sulfate for water collection structure 74 in red disperse dye componen

References:

CN105440727,2016,A Location in patent:Paragraph 0042; 0043; 0044; 0045