- Synthesis method of chronic granulocytic leukemia treating medicinal intermediate
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The invention relates to a synthesis method of a chronic granulocytic leukemia treating medicinal intermediate. The synthesis method comprises the following steps: (a), dissolving trichloroacetaldehyde hydrate by using water, sequentially adding an aqueous solution of anhydrous sodium sulfate, a hydrochloric acid solution of 3, 4-dimethoxyaniline and an aqueous solution of hydroxylamine hydrochloride, filtering and drying to obtain a compound 2; (b), mixing the compound 2 and polyphosphoric acid to obtain a compound 3; (c), dissolving the compound 3 and rhodanine by using pyridine, and dryingto obtain a compound 4; (d), mixing the compound 4 and a KOH solution, heating to 40-60 DEG C, reacting while stirring, and drying to obtain a compound 5. By the synthesis method, synthesis of a key intermediate of an indirubin derivative can be achieved, the yield and the purity are relatively high, and industrial batch production is facilitated.
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Paragraph 0016; 0119; 0024
(2018/09/08)
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- Method for synthesizing drug for treating chronic granulocytic leukemia
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The invention relates to a method for synthesizing a drug for treating chronic granulocytic leukemia. The method comprises the following steps: (a) dissolving a chloral hydrate with water, sequentially adding an aqueous solution of anhydrous sodium sulfate, a hydrochloric solution of 3,4-dimethoxyaniline and an aqueous solution of hydroxylamine hydrochloride, and performing filtering and drying, so as to obtain a compound 2; (b) mixing the compound 2 with polyphosphoric acid, so as to obtain a compound 3; (c) dissolving the compound 3 and rhodanine with pyridine, and carrying out drying, so asto obtain a compound 4; (d) mixing the compound 4 with a KOH solution, then, heating the temperature of the mixture to 40 DEG C to 60 DEG C, carrying out a reaction with stirring, and carrying out drying, so as to obtain a compound 5; (e) mixing the compound 5 with aniline, then, carrying out a reaction with stirring at the temperature of 100 DEG C to 150 DEG C under nitrogen protection, and carrying out drying, so as to obtain a compound 6; (f) heating the temperature of polyphosphoric acid to 100 DEG C to 150 DEG C, adding the compound 6 under the condition of continuous stirring, carryingout a reaction, and carrying out purification, thereby obtaining the drug. Thus, indirubin derivatives can be synthesized and have relatively high yield and purity, and the industrialized mass production is facilitated.
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Paragraph 0018; 0021; 0027
(2018/09/11)
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- Synthesis method for final intermediate of chronic granulocytic leukemia drug
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The invention relates to a synthesis method for a final intermediate of a chronic granulocytic leukemia drug. The method comprises the steps of: (a) dissolving a trichloracetic aldehyde hydrate in water, then adding an aqueous solution of anhydrous sodium sulfate, a hydrochloric acid solution of 3, 4-dimethoxyaniline and an aqueous solution of hydroxylamine hydrochloride in order, and conducting filtering and drying to obtain a compound 2; (b) mixing the compound 2 with polyphosphoric acid to obtain a compound 3; (c) dissolving the compound 3 and rhodanine in pyridine, and performing drying toobtain a compound 4; (d) mixing the compound 4 with a KOH solution, then performing heating to 40-60DEG C, carrying out stirring reaction, and performing drying to obtain a compound 5; and (e) mixingthe compound 5 with aniline, then carrying out stirring reaction at 100-150DEG C under nitrogen protection; and performing drying to obtain a compound 6. The method provided by the invention can realize synthesis of indirubin derivative intermediates with high yield and purity, and is conducive to industrial batch production.
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Paragraph 0017; 0020; 0026
(2018/09/12)
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- A novel strategy to the synthesis of 4-anilinoquinazoline derivatives
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A novel approach to prepare 4-anilinoquinazoline derivatives based on the transformation of indoline-2,3-dione to formamidine was developed. The processes with this approach are simple, efficient, and environmentally friendly. The efficiency of this approach was evaluated by synthesizing 17 4-anilinoquinazolines and comparing the obtained yields with those achievable through conventional synthetic methods. It was the first time that compounds 8d, 8e, 8h, and 13b-f were synthesized. The characteristics of the IR and the UV spectra of these compounds and the effects of their substituents on the spectra were observed.
- Wang, Zheng,Wang, Cuiling,Sun, Yanni,Zhang, Ning,Liu, Zhulan,Liu, Jianli
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p. 906 - 913
(2014/01/23)
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- Synthesis and biophysical evaluation of arylhydrazono-1H-2-indolinones as β-amyloid aggregation inhibitors
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A series of isatin-3-arylhydrazones were synthesized and evaluated in vitro as inhibitors of Aβ1-40 aggregation using a thioflavin T fluorescence method. An exploration of the effects on Aβ1-40 aggregation of a number of diverse subs
- Campagna, Francesco,Catto, Marco,Purgatorio, Rosa,Altomare, Cosimo D.,Carotti, Angelo,De Stradis, Angelo,Palazzo, Gerardo
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scheme or table
p. 275 - 284
(2011/02/27)
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- A new approach to methoxyisatins leading to the total synthesis of ophiuroidine and other hydroxytryptanthrins
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A new method for the preparation of methoxyisatins from the corresponding methoxyanilines is described. The resulting methoxyisatins were used in the syntheses of several methoxytryptanthrin compounds. The natural product ophiuroidine (4,8,9-trihydroxytry
- Mason, Jeffrey J.,Janosik, Tomasz,Bergman, Jan
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experimental part
p. 3642 - 3648
(2010/03/05)
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- Combinatorial optimization of isatin-β-thiosemicarbazones as anti-poxvirus agents
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Novel strategies are required to combat pox virus infections, whether caused by escape of viruses such as monkeypox from indigenous areas or intentional release of smallpox. Anti-smallpox drugs with a unique mode of antiviral action, inhibition of transcription termination, were known but not therapeutically useful. Using a combinatorial method, variants of the basic isatin-β-thiosemicarbazone structure were prepared and examined for cytotoxicity and antiviral activity in vaccinia virus- and cowpox virus-infected human cells. Potent and much more selective N-aminomethyl-isatin-β- thiosemicarbazones were discovered.
- Pirrung, Michael C.,Pansare, Sunil V.,Das Sarma, Koushik,Keith, Kathy A.,Kern, Earl R.
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p. 3045 - 3050
(2007/10/03)
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- Synthesis of Dopamines Labelled with 13C in the α- or β-Side Chain Position and Their Application to Structural Studies on Melanins by Solid-State NMR Spectroscopy
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Solid-state NMR spectroscopy was applied to the analysis of melanins prepared by peroxidase-H2O2 oxidation of dopamines specifically 13C labelled in the α- or β-side chain positions.A surprisingly diverse pattern of signals indicated the presence of uncyclized dopamine and noradrenaline-derived units, in addition to indole and carbonyl carbon atoms.These structural features, coupled with the results obtained from elemental analysis of dopamine melanin samples prepared under different conditions, point to a pigment formation process more complex than previously believed. - Key Words: CP-MAS NMR Spectroscopy / Melanin / Oxidative phenolic coupling / Quinone methides / Labelled compounds, 13C / Dopamines / Enzymes
- Crescenzi, Orlando,Kroesche, Christoph,Hoffbauer, Wilfried,Jansen, Martin,Napolitano, Alessandra,et al.
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p. 563 - 568
(2007/10/02)
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- PHOTO-OXIDATION OF 5,6-DIHYDROXYINDOLES
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The photo-oxidative behaviour of some 5,6-dihydroxyindoles (1-6) in organic solvents with Pyrex-filtered UV light has been investigated.In methanol, all the indoles exhibited a marked tendency to undergo photodecomposition giving very complex mixtures of products.In the case of 5,6-dimethoxyindole, 5, work-up of the reaction mixture led to isolation of two main photo-oxygenation products which were identified as the isatin 7 and the ring-opened derivative 8 by spectral analysis.The use of acetone as solvent markedly altered the reaction cource, causing cleavage of the C2-C3 bond in all the indoles examined, including the parent ring system, to give N-formylanthranilic acid in good yields.
- d'Ischia, Marco,Prota, Giuseppe
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p. 407 - 410
(2007/10/02)
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- The Synthesis of the Dimethoxyisatins
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Preparations of all 6 dimethoxyisatins are described.The methods of synthesis of these compounds from anilines have been compared, the route via the 3-(methylthio)oxindoles giving, in general, the best yield.These isatins are strikingly different in colou
- Taylor, A.
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p. 4154 - 4171
(2007/10/02)
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