| production method | 1. The 4,4 '-oxobisbenzenesulfonyl chloride obtained by sulfonyl chlorination of diphenyl ether with chlorosulfonic acid is then reacted with hydrazine hydrate to give 4,4'-oxobisbenzenesulfonyl hydrazine. The reaction scheme is as follows: the reaction between diphenyl ether and excess chlorosulfonic acid (molar ratio of about 1:6) was carried out at room temperature for 2 hours and then poured into water for filtration to obtain crude intermediate 4,4 '-chlorobenzenesulfonyl chloride. The diphenyl ether is sulfonated with approximately equal amount of concentrated sulfuric acid under vacuum at 135 ℃ for 4H, then refluxed with equal amount of phosphorus oxychloride for 3H, poured into ice water, precipitated, filtered, washed with water, filtration and drying gave the intermediate. The intermediate was reacted with a slight excess of hydrazine hydrate and an equivalent amount of aqueous ammonia at 30-40 °c for 3H, and finally filtered, washed with water and dried to obtain the product. 2. The diphenyl ether is first sulfonated with concentrated sulfuric acid, and then reacted with phosphorus oxychloride to obtain 4,4 '-oxobisbenzenesulfonyl chloride, which is further reacted with hydrazine hydrate and ammonia water to obtain 4,4'-oxobisbenzenesulfonyl hydrazine. The reaction scheme is as follows: a predicted amount of diphenyl ether and concentrated sulfuric acid are added to the reaction flask. The reduced pressure system is switched on and the temperature is slowly increased to 135 °c. After the reaction was maintained for 4H, the temperature was lowered to 100-110 ℃, and the decompression system was removed. The expected amount of phosphorus oxychloride was added dropwise from the dropping funnel, and the reaction was maintained for about 3H before cooling. The reactants were precipitated in ice water. After washing the precipitated product, a certain amount of precipitated product was placed in another reaction bottle, and a certain amount of water was added to start stirring. A mixture of aqueous ammonia and hydrazine hydrate was added and the reaction was maintained at 40 °c. After about 3H, the reaction was filtered, washed with water until neutral, and dried under vacuum or IR to give an off-white powder product. |