- Preparation method of chlorquinaldol
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The invention provides a preparation method of chloroquinaldoll. The preparation method comprises the following step: in the presence of a catalyst Lewis acid, carrying out a reaction I on a material containing 8-hydroxy-2-methylquinoline and tert-butyl hypochlorite to obtain the chloroquinaldol. According to the method, the tert-butyl hypochlorite is used for replacing chlorine to serve as a reaction raw material, so good selectivity is achieved, byproducts are few, reaction operability is strong, light shielding and gas protection are not needed, quality and yield are improved, the purity of chlorquinaldol is 99.00% or more, and the quality of chlorquinaldol is ensured. In the reaction process, generation of waste liquid is reduced, pollution to the environment is avoided to the maximum extent, cost is saved, quality is improved, and the method is an environment-friendly process suitable for industrial production.
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Paragraph 0066-0093
(2021/10/27)
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- Preparation method of chlorquinaldol
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The invention provides a preparation method of chlorquinaldol. The preparation method comprises the following step: in the presence of a catalyst Lewis acid, subjecting a material I containing 8-hydroxy-2-methylquinoline and dichlorohydantoin to reacting so as to obtain the chlorquinaldol. According to the invention, dichlorohydantoin is used as a reaction raw material to replace chlorine, so good selectivity is achieved, byproducts are few, reaction operability is strong, light shielding and gas protection are not needed, quality and yield are improved, the purity of chlorquinaldol is 99.00% or more, and the quality of chlorquinaldol is ensured. In the reaction process, generation of waste liquid is reduced, pollution to the environment is avoided to the maximum extent, cost is saved, quality is improved, and the method is an environment-friendly process suitable for industrial production.
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Paragraph 0063-0090
(2021/10/27)
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- Preparation method of chloroquinaldol
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The invention belongs to the technical field of medicines, and particularly relates to a preparation method of chloroquinaldol. The preparation method comprises the following steps: adding water intochloroquinaldol hydrochloride for dissolving, adding a buffer solution under the conditions of light shielding and nitrogen protection, regulating the pH value by using alkali, filtering and refiningthe solution to obtain chloroquinaldol. The method is easy and convenient to operate and suitable for industrial production, the purity of the prepared chloroquinaldol is high and can reach 99.99% orabove, and the stability of the product is high.
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Paragraph 0034-0047
(2020/05/30)
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- Rare earth complex constructed based on 2- methyl -5,7- dichloro -8- hydroxyquinoline, and preparation method and application thereof
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The rare earth complex constructed based on 2 - methyl - 55557-dichloro - 8 8-hydroxyquinoline and a preparation method and application. of the rare earth complex are respectively a complex 1 and a complex 2, complex 1. [Er(ClQ). 3 (H2 O)], Complex 2 has a molecular formula of [Ho(ClQ). 3 (H2 A test result of O)], ClQ of 2 - methyl - 55557-dichloro - 8 8-dichloro - 8 8-hydroxyquinoline and erbium nitrate hexahydrate or holmium nitrate hexahydrate, are reacted. under a heating condition of: respectively. 2 - The test result shows, that the rare earth complex has a remarkable anti-proliferative effect on a plurality of tumor cells, and is expected to be developed into anti-tumor medicines pH＝7.7 - 8.2 by using, a mixed solvent dissolving, at a heating condition.
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Paragraph 0022-0024
(2020/03/25)
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- To 2 - methyl - 5, 7 - dichloro -8 - hydroxy quinoline as ligands of the single nucleus arrowhead complex and its preparation method and application
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The invention discloses a mononuclear dysprosium complex using 2-methyl-5,7-dichloro-8-hydroxyquinoline as a ligand and a preparation method and application thereof. A chemical formula of the complex is: [Dy(L)3(HL)], wherein L represents a product obtained after hydrogen atom of hydroxyl is removed from 2-methyl-5,7-dichloro-8-hydroxyquinoline, and has one unit of negative charges; HL represents 2-methyl-5,7-dichloro-8-hydroxyquinoline; the complex belongs to a triclinic system and a P-1 space group. The preparation method of the complex, which is disclosed by the invention, comprises: taking Dy(NO3)3.6H2O and 2-methyl-5,7-dichloro-8-hydroxyquinoline; dissolving Dy(NO3)3.6H2O and 2-methyl-5,7-dichloro-8-hydroxyquinoline with methanol; regulating pH of the obtained solution into a range of 6.5 to 7.8; performing a reaction on the obtained mixed solution under the heating condition to obtain the mononuclear dysprosium complex. The complex provided by the invention is simple in preparation method, low in cost and good in repeatability, shows a field-induced slow relaxation magnetic behavior at a low temperature, and can be used for preparing a magnetic material.
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Paragraph 0028; 0029
(2019/02/19)
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- Synthetic technology of chlorquinaldol
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The invention belongs to the field of pharmaceutical synthesis technology and specifically relates to a synthetic technology of chlorquinaldol. By using Lewis acid as a catalyst, 8-hydroxy-2-methylquinoline and N-Chlorosuccinimide, which are used as raw materials, are subjected to a one-step chlorination reaction to generate chlorquinaldol; and after the reaction, chlorquinaldol is refined to obtain the chlorquinaldol. By using N-Chlorosuccinimide to replace chlorine as the raw material of the chlorination reaction, the selectivity is good, side reaction is reduced, conversion rate and yield are increased, yield reaches 98.2% and above, purity is 99.90% and above, quality of the chlorquinaldol is guaranteed, generation of spend liquor is decreased, environmental pollution is reduced, the cost is saved, water dissolution of the reaction product is avoided, and the yield is increased. The technology of the invention is a green and environmentally-friendly technology, and is suitable forindustrial production.
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Paragraph 0026-0035
(2019/08/30)
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- Process for synthesizing chlorquinaldol
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The invention belongs to the technical field of medicine synthesis, and particularly relates to a process for synthesizing chlorquinaldol. The process comprises the following steps: carrying out reaction between 8-hydroxyl-2-methylquinoline as a raw material and sodium hypochlorite and hydrochloric acid to generate active chlorine atoms as a chlorinated material; performing one-step chlorinated reaction to generate the chlorquinaldol. According to the process disclosed by the invention, using chlorine as a chlorinated material is avoided, and chlorquinaldol is quantitatively generated, so thatthe selectivity and the yield of chlorinated reaction are improved, and meanwhile, the phenomena that pollution on the environment by adopting the chloride and side reaction caused by performing thechlorinated reaction adopting the chloride as the chlorinated material are avoided, and the quality of the chlorquinaldol is ensured.
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Paragraph 0018-0032
(2018/09/08)
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- Mononuclear dysprosium complex using 2-methyl-5,7-dichloro-8-hydroxyquinoline as ligand and preparation method and application thereof
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The invention discloses a mononuclear dysprosium complex using 2-methyl-5,7-dichloro-8-hydroxyquinoline as ligand and a preparation method and application thereof. The chemical formula of the complex is [Dy(L)4].(H2O)(DMF)(HN(C2H5)3), wherein L represents 2-methyl-5,7-dichloro-8-hydroxyquinoline without hydroxyl hydrogen atoms and provided with a unit of negative charges, DMF is N,N-dimethylformamide, and the complex belongs to a P21/n space group of a monoclinic crystal system. The complex is obtained by dissolving Dy(NO3)3.6H2O and the 2-methyl-5,7-dichloro-8-hydroxyquinoline with mixed solvents, regulating the pH of the obtained solution to be 6.5 to 7. 8 and making the mixed solution react under the heating conditions. The preparation method of the complex is simple, cheap and good in repeatability, shows field induced slow relaxation magnetic behavior at low temperature and can be used for preparing magnetic materials.
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Paragraph 0029; 0030
(2017/08/29)
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- Based on 2 - methyl - 5, 7 - dichloro - 8 - hydroxy quinoline as ligands of the single nucleus arrowhead complex and its preparation method and application (by machine translation)
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The invention discloses a method based on 2 - methyl - 5, 7 - dichloro - 8 - hydroxy quinoline as ligands of the single nucleus arrowhead complex and its preparation method and application. The complex chemical formula is: [Dy (L)3 (H2 O)], wherein L is 2 - methyl - 5, 7 - dichloro - 8 - hydroxy quinoline hydroxyl group to hydrogen atom, with a unit of negative charge; this complex belongs to the triclinic system, P - 1 space group. The invention for the preparation of the complexes: taking Dy (NO3 )3 · 6 H2 O and 2 - methyl - 5, 7 - dichloro - 8 - hydroxy quinoline, dissolved in water, the resulting solution to adjust the pH=6.5 - 7.8, the mixed liquid obtained by reaction under heating condition, to obtain. The present invention provides a complex preparation method is simple, low cost, repeatability is good, at the low temperature performance is field-induced slow relaxation magnetism acts, can be used for preparing magnetic material. (by machine translation)
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Paragraph 0028; 0029
(2017/09/26)
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- Direct, catalytic, and regioselective synthesis of 2-alkyl-, aryl-, and alkenyl-substituted N -Heterocycles from n -oxides
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A one-step transformation of heterocyclic N-oxides to 2-alkyl-, aryl-, and alkenyl-substituted N-heterocycles is described. The success of this broad-scope methodology hinges on the combination of copper catalysis and activation by lithium fluoride or magnesium chloride. The utility of this method for the late-stage modification of complex N-heterocycles is exemplified by facile syntheses of new structural analogues of several antimalarial, antimicrobial, and fungicidal agents.
- Larionov, Oleg V.,Stephens, David,Mfuh, Adelphe,Chavez, Gabriel
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supporting information
p. 864 - 867
(2014/03/21)
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- 3-Imino-1,2,4-benzotriazine-1-oxides
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New 3-Imino-1,2,4-benzotriazine-1-oxides of formula I SPC1 wherein R represents an alkyl, alkenyl or haloalkyl radical, a phenyl or aralkyl radical optionally substituted by alkyl, alkoxy, haloalkyl, halogen or hydroxy, X and Y each independently represent hydrogen, halogen, an alkyl or alkoxy radical, or one of the two symbols represents a phenoxy or phenylsulphonyl radical optionally substituted by halogen, alkyl, haloalkyl and/or alkoxy which are active against harmful microorganisms are disclosed.
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