4-NITROAZOBENZENE TECH. 90 synthesis
- Product Name:4-NITROAZOBENZENE TECH. 90
- CAS Number:2491-52-3
- Molecular formula:C12H9N3O2
- Molecular Weight:227.22
34139-26-9
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2491-52-3
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$70.00/500mg
Yield:2491-52-3 196 g
Reaction Conditions:
with sodium hypochlorite in dichloromethane at 20; for 6 h;Green chemistry;
Steps:
1 Preparation process:
In a reaction vessel equipped with a stirring and a thermometer, 1.0 mol of phenylhydrazine (108.1 g), 500 ml of dichloromethane, and 8 g of potassium carbonate-modified alumina solid base were successively added, and the temperature was controlled at 20-40 ° C.1.05 mol of 4-nitrochlorobenzene (165.4 g) was added dropwise, and the reaction vessel was placed under an ultrasonic condition at 38-40 ° C for 1 hour. The solid was removed by filtration, and the filtrate was added to 200 ml of a 10 wt% sodium hypochlorite solution, and the reaction was stirred at room temperature for 6 hours, and the mixture was allowed to stand for separation, the aqueous phase was removed, and the dichloromethane layer was concentrated to give a crude product. The crude product was recrystallized from dichloromethane to give 196 g of 4-nitrophenylazobenzene with a purity of 98.8% (total yield 86.3%). The recovered dichloromethane can be recycled for use.
References:
CN104230747,2019,B Location in patent:Paragraph 0032-0036
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2491-52-3
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2491-52-3
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2491-52-3
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