ChemicalBook CAS DataBase List 2-amino-3,5-dinitrobenzonitrile

2-amino-3,5-dinitrobenzonitrile synthesis

11synthesis methods

Product Name:2-amino-3,5-dinitrobenzonitrile
CAS Number:22603-53-8
Molecular formula:C7H4N4O4
Molecular Weight:208.13

19019-04-6
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22603-53-8
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Yield:22603-53-8 84.5%

Reaction Conditions:

with ammonia in chlorobenzene at 110 - 120; under 11251.1 - 13501.4 Torr; for 5 h;Autoclave;Pressure;Temperature;Solvent;

Steps:

1-4

120 g of the second intermediate 2-methoxy-3,5-dinitrobenzonitrile and 350 g of chlorobenzene were added to a 1 L autoclave.Add 135 g of liquid ammonia, the reaction temperature is 110-120 ° C, and the pressure is about 1.5-1.8 MPA.The reaction time is 5 hours. After the reaction is finished, the temperature is released at room temperature, and the mother liquor is filtered to obtain crude 2-amino-3,5-dinitrobenzonitrile.The filtrate is rectified to recover chlorobenzene and by-product methanol.The crude product is detected by HPLC, the content is ≥97%, and it can reach 98.5% or more with a little refinement.The ammoniation yield was 84.5% and the product was yellow crystals.

References:

CN110294691,2019,A Location in patent:Paragraph 0031; 0034-0036; 0039-0040; 0043-0044; 0047