DISPERSE ORANGE 3 synthesis
- Product Name:DISPERSE ORANGE 3
- CAS Number:730-40-5
- Molecular formula:C12H10N4O2
- Molecular Weight:242.23
Yield:730-40-5 97.1%
Reaction Conditions:
Stage #1:1,4-phenylenediamine with hydrogenchloride;sodium nitrite in water at -5 - 0; for 1 h;
Stage #2: with urea in water for 0.5 h;
Stage #3:4-nitro-aniline with hydrogenchloride in water for 0.5 h;
Steps:
2 2) 4- (4'-Nitro-azobenzene) -anilineSynthesis
To a flask equipped with a mechanical stirrer,Thermometer in a 500 ml three-necked flaskThe p-phenylenediammonium product obtained in Step 1) was addedAnd 250.0 ml of dilute hydrochloric acid at a concentration of 5 mol / L,While cooling to a temperature of -5 ° C - 0 ° C,A 7.11 g (0.103 mol) aqueous solution of sodium nitrite dissolved in 40.0 ml of water was slowly added dropwise with a constant-pressure dropping funnel,The dropping process kept the temperature at -5 ° C to 0 ° C,After completion of the drop in 0 - 5 ° C heat 60 minutes of stirring,10 g (0.166 mol) of urea dissolved in 40.0 ml of water was added,Stirred for 0.5 hour,14.35 g (0.104 mol) of p-nitroaniline was added dropwiseDissolved in 50.0ml5mol / L dilute hydrochloric acid solution,After completion of the addition, the reaction was continued for 0.5 hour,The low temperature was neutralized with saturated potassium carbonate solution,filter,A precipitate,Vacuum drying,To obtain the product of 4- (4'-nitro - azobenzene) - aniline 24.44 g (0.101mol),Yield 97.1%.
References:
Yantai Xianhua Chem-Tech Co., Ltd.;Wang, Peixiang;Liu, Lu;Tang, Zhilin;Fang, Fengmei;Xu, Liang;Li, Meihua CN105348849, 2016, A Location in patent:Paragraph 0048; 0049
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