85-48-3Relevant articles and documents
Preparation method of 8-hydroxyquinoline
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Paragraph 0042; 0043; 0045; 0046; 0048; 0049, (2018/03/26)
The invention relates to a preparation method of 8-hydroxyquinoline. The preparation method comprises the following steps: A), uniformly mixing quinoline and a sulfonating agent, performing a sulfonation reaction, and hydrolyzing to obtain a reaction solid and reaction liquid; B), under the action of a catalyst, heating the reaction solid obtained in the step A), water and inorganic strong alkali,and reacting to obtain the 8-hydroxyquinoline, wherein the catalyst is one or more of methanol, ethanol and isopropanol. By the preparation method, through addition of the catalyst during the reaction, the reaction temperature in an alkali-melting step in the production process of the 8-hydroxyquinoline is reduced, so that a requirement on equipment is reduced and the danger coefficient in actualproduction is also reduced, and thus a reaction condition is mild, operation is easy, and the purity and the yield are relatively high; meanwhile, through the addition of the catalyst, the using amount of the inorganic strong alkali is reduced, so that the production cost is reduced; in addition, the reaction liquid produced in the sulfonation reaction is recycled in a subsequent acidification process, so that discharge of waste liquid is reduced and clean production is achieved.
A 8-hydroxy quinoline synthesis method (by machine translation)
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Paragraph 0020; 0021; 0022; 0023; 0024, (2016/10/31)
The present invention provides a kind of 8-hydroxy quinoline synthesis method, the steps are as follows : (1) added to the fuming sulfuric acid in four-mouth bottle, actuated stirring, 12 °C the quinoline is put into the constant pressure dropping funnel, and then the quinoline dropping slowly added in four-mouth bottle, completion of the postheating to 90-110°C, thermal insulation sulfonated 3 hours ; (2) the solution in the tube is moved to the radiation, nitrogen 30 minutes and then closed, the irradiation in a cobalt source 2 hours, the solution is taken out after, adding ice water for dilution, frozen 1 day, to crystallize, filtering, drying to obtain 8-sulfonic acid quinolines ; (3) in the four bottle by the addition of a base, heating to 260-320 °C enable its fusing, adding stirring 8-sulfonic acid quinolines, thermal insulation reaction 3 hours, the temperature after the completion of the 90 °C, adding distilled water to make its full dissolved, cooling to room temperature, neutralized to the solution for PH 7, after filtration of the precipitated crystals of distillation, to obtain white crystalline solid 8-hydroxy quinoline. The operation of the invention is simple, low cost, high yield. (by machine translation)
A convenient synthesis of novel 3-(heterocyclylsulfonyl)propanoic acids and their amide derivatives
Dorogov, Mikhail V.,Filimonov, Sergey I.,Kobylinsky, Dmitry B.,Ivanovsky, Sergey A.,Korikov, Pavel V.,Soloviev, Mikhail Y.,Khahina, Maria Y.,Shalygina, Elena E.,Kravchenko, Dmitry V.,Ivachtchenko, Alexandre V.
, p. 2999 - 3004 (2007/10/03)
A large number of novel 3-(heterocyclylsulfonyl)propanoic acids and their amide derivatives were prepared in good yields and excellent purity starting from the corresponding heterocyclic compounds. At first, chlorosulfonates were generated by reaction of initial heterocycles with various sulfonating and chlorinating agents followed by their conversion into sodium sulfinates. Treatment of sulfinates with acrylic acid smoothly afforded a series of sulfonylpropionates, which were used as convenient reagents for the preparation of a large number of the corresponding carboxamide derivatives.