ChemicalBook CAS DataBase List Dibenzenesulfonimide

Dibenzenesulfonimide synthesis

8synthesis methods

Product Name:Dibenzenesulfonimide
CAS Number:2618-96-4
Molecular formula:C12H11NO4S2
Molecular Weight:297.35

Manufactured by treating benzene- sulfonamide in 5% sodium hydroxide solution with benzenesulfonyl chloride at 50 – 55 ℃ (1 – 2 h). During the reaction the pH value must be kept at 7.2 by adding 5% sodium hydroxide solution. At the end of the reaction the disulfonylamine is precipitated from the clear solution by adding hydrochloric acid. Yield: 70 – 98%

98-10-2 Synthesis

98-10-2
328 suppliers
$18.00/25g

98-09-9
341 suppliers
$12.00/25g

2618-96-4
283 suppliers
$6.00/5g

Yield:2618-96-4 93%

Reaction Conditions:

with sodium hydroxide at 60;Concentration;

Steps:

6 Example 6

A solventless grinding method for preparing bis-benzenesulfonimide,First 500 grams (3.185 mol) of benzenesulfonamide and 1009 grams were added(5.733 mol) of pure benzenesulfonyl chloride into a volume of 5Liter stainless steel ball mill for 5 minutes,The benzenesulfonamide and benzenesulfonyl chloride are thoroughly mixed at room temperature;Then in 5 times to the stainless steel ball mill 255 g (6.37 mol)Solid NaOH, the material after each addition of NaOH grinding 3 to 7 minutes,And keep the temperature of the reactants below 60 ° C for 15 minutes;After the reaction was completed, the reaction was transferred from the ball mill to a 5-liter three-necked flask,The reaction was added 10 times the mass of methylene chloride,Install the condenser, heating, stirring, reflux for 30 minutes, hot filtration,The solid in the funnel was washed three times with hot methylene chloride,The generated NaCl was filtered off and the filtrate was combined; Finally, the filtrate was concentrated under heating at atmospheric pressure,After evaporating 2/3 of the solvent, the remaining material was cooled at room temperature,After crystallization, filtration, to give a precipitate,The precipitate was dried at a temperature of 85 ° C,That is, bisbenzenesulfonimide product 879 grams, the yield was 93%Purity 98.0%.

References:

CN106631916,2017,A Location in patent:Paragraph 0018; 0019; 0020; 0021; 0022; 0023; 0024-0027