4,4'-Bis(chlorosulfonyl)diphenyl ether synthesis

Yield:-

Reaction Conditions:

Stage #1: diphenyletherwith sulfuric acid at 60 - 132; for 2.41667 h;
Stage #2: with trichlorophosphate at 105; for 1.83333 h;Temperature;

Steps:

4.4

35 g of diphenyl ether was added to a four-necked flask and heated to 60 ° C with stirring, Then, under the condition of negative pressure, 97.89% concentrated sulfuric acid (30g) was added dropwise, and the time was added dropwise for 25 minutes. When concentrated sulfuric acid is added, the temperature is raised to 132 ° C at 132 ° C, Negative pressure and stirring conditions to make concentrated sulfuric acid and diphenyl ether to keep the reaction 2h, To obtain a sulfonic acid mixture of diphenyl ether-4-sulfonic acid and diphenyl ether-4,4'-disulfonic acid; at a temperature of 0 - 5 °C and stirring condition, to the sulfonic acid is added in the mixture 35g anhydrous ethanol, sodium hydroxide for adjusting the pH value of the system 7, then filtered, the solid salt is diphenyl ether disulfonic acid sodium, In the temperature of 105 ° C and stirring conditions, add phosphorus oxychloride 58.46 grams, dropping time 20 minutes, after the drop is completed, And then 105 ° C temperature conditions to diphenyl ether sulfonic acid and phosphorus oxychloride continue to heat for 1.5h, After the reaction, the reaction product containing the solid target product is obtained, the reaction product is washed with water to obtain the solid target product, The solid target product is 4,4'-oxydi(phenylsulfonyl chloride

References:

CN106588703,2017,A Location in patent:Paragraph 0018-0023