81-08-3Relevant articles and documents
Preparation method of acyl sulfonate compounds
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Paragraph 0064-0069; 0087, (2021/01/29)
The invention belongs to the field of chemical engineering, and discloses a preparation method of acyl sulfonate compounds. The method comprises the following steps: (1) carrying out sulfonyl chlorination or sulfonation on a sulfydryl-containing compound in an organic solvent under the action of an acylating chlorination reagent, and separating by using a rectification, extraction or sedimentationmethod to obtain sulfonyl-chlorinated or sulfonated products; (2) condensing the sulfonyl-chlorinated or sulfonated compounds and a carboxyl-containing compound to prepare acyl sulfonate compound crude products; and (3) washing the acyl sulfonate compound crude products obtained in the step (2) by using a low-boiling-point solvent to obtain the purified acyl sulfonate compounds. According to themethod, the adopted raw materials are simple and easy to obtain, the cost is low, the synthesis route is simple, the conditions are mild, the reaction activity is high, the reaction conversion rate isup to 90% or above, and the purity of various prepared acyl sulfonate compounds is high.
Synthesis process of sulfonic-group rhodamine compound
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Paragraph 0027-0029; 0033; 0034; 0038; 0039; 0043; 0044, (2019/04/26)
The invention discloses a synthesis process of a sulfonic-group rhodamine compound. The process comprises the steps: mixing saccharin and a protonic acid catalyst, performing heating for a reaction soas to obtain a compound shown in a formula (I), performing a reaction between a compound shown in a formula (II) and resorcinol through heating under the action of the protonic acid catalyst so as toobtain a compound shown in a formula (III), performing a reaction between the compound of the formula (I) and the compound in the formula (III) through heating under the action of a Lewis acid catalyst under the conditions of nitrogen protection and light shielding so as to obtain the sulfonic-group rhodamine compound shown in a formula (IV). Through the synthesis process, the use of thionyl chloride in a conventional process is avoided, the operation is simplified, the production safety is improved, the pollution to the environment is little, the reaction can be carried out under normal pressure, and the reaction has a high selectivity; and the chemical structural formulas of the compounds represented separately by the formula (I), the formula (II), the formula (III) and the formula (IV)are shown.
Synthesis of a few cyclothiadiazanones and aminosulfonyl benzamides from saccharin
Ramana, P. Venkata,Reddy, A. Ram
experimental part, p. 71 - 81 (2010/10/04)
Saccharin is hydrolyzed with two different acids to yield 1,2-di-acid. The di-acid, on chlorination with phosphorous pentachloride, gave 2-chlorosulfonylbenzoyl chloride. The 2-chlorosulfonylbenzoyl chloride on hydrazinolysis gave benzothiadiazinetrione, while with phenyl hydrazine it selectively yielded 2-phenylbenzothiadiazinetrione. 2-chlorosulfonoylbenzoyl chloride with different aromatic 1,2- diamines resulted in dibenzothiadiazocine derivatives. Electron-donating groups in the diamine facilitate while the electron-withdrawing groups retard the cyclization. However, aliphatic diamines, aniline and substituted anilines readily gave acyclic aminosulfonyl carboxybenzamides on condensation with 2- chlorosulfonylbenzoyl chloride. The di-acid and anhydride did not react with either hydrazine/phenyl hydrazine or amines to give the above products. However, when its ester derivative, isopropyl-2- chlorosulfonylbenzoate, condensed with hydrazine, it gave benzothiadiazinetrione. But the ester failed to react with phenyl hydrazine. All the condensation reactions were carried out at room temperature.