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Benzene, 2,4-difluoro-1,3,5-trinitro- synthesis

2synthesis methods
1630-09-7 Synthesis
1,3-DICHLORO-2,4,6-TRINITROBENZENE

1630-09-7
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Yield:784-12-3 75.1%

Reaction Conditions:

with potassium fluoride;18-crown-6 ether in neat (no solvent) at 70 - 75;Catalytic behavior;

Steps:

12 Preparation of 2,4-difluoro-1,3,5-trinitrobenzene

Add 282.0g 2,4-dichloro-1,3,5-trinitrobenzene, 282.0g 18-crown-6 and 133.6g anhydrous potassium fluoride to a 1L reaction flask, and heat to 70-75C for reaction 5 ~8 hours, after the central control reaction is complete, the temperature is lowered, filtered, the filter cake is slurried with toluene, the organic phases are combined, and the toluene is recovered by short evaporation. The resulting still residue is recrystallized with ethanol to obtain 186.8g of product, the yield is 75.1%, and the HPLC purity is 98.0 %. After the crystallization mother liquor is concentrated, 302.9 g of the kettle residue is obtained.

References:

CN112939782,2021,A Location in patent:Paragraph 0184-0191