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ChemicalBook CAS DataBase List bis(4-chloro-3-nitrophenyl) sulphone
1759-05-3

bis(4-chloro-3-nitrophenyl) sulphone synthesis

3synthesis methods
-

Yield:1759-05-3 99%

Reaction Conditions:

with sulfuric acid;nitric acid in 1,2-dichloro-ethane;

Steps:

1 EXAMPLE 1

EXAMPLE 1 57.4 g (0.2 moles) of 4,4'-dichloro diphenylsulfone is dissolved in 170 ml of 1,2-dichloro ethane. Following addition of 28.2 g of nitric acid (specific gravity 1.50) at room temperature, to the resultant mixture there is added 98% sulfuric acid dropwise during 30 minutes at 30°-40° C. After stirring for 7 hours at 70°-80° C., the mixture is cooled and then separated into an organic layer and a mixed acid layer. The solvent is removed by steam distillation. The precipitate is filtered, washed with water and dried to give needle-like crystals of 3,3'-dinitro-4,4'-dichloro diphenylsulfone (74.6 g). Yield 99%. Purity determined by high performance liquid chromatography is 99.6%. Melting point 201°-202° C. By recrystallization from ethanol there is obtained needle-like pure crystals. M.P. 201°-202° C.

References:

US4482742,1984,A

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