ChemicalBook CAS DataBase List 4-NITROAZOBENZENE TECH. 90

4-NITROAZOBENZENE TECH. 90 synthesis

8synthesis methods

Product Name:4-NITROAZOBENZENE TECH. 90
CAS Number:2491-52-3
Molecular formula:C12H9N3O2
Molecular Weight:227.22

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2491-52-3
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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

60-11-7 Synthesis