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Preparation technology for crystal of dithiole pyrrolones compound
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A technology of dithiocyclopentene and dithiocyclopentene, applied in the field of chemistry, can solve problems such as difficulty in absorption and utilization, poor water solubility, and inability to fully exert the curative effect of drugs
Active Publication Date: 2013-12-18
魏爽
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Problems solved by technology
However, at present, the compound products refined by known techniques all exist in the form of yellow cotton flocs. Due to the poor water solubility of the known crystal form of the compound, it is difficult to absorb and utilize it in the human body when used as a drug. , can not give full play to the efficacy of the drug
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Embodiment 1
[0023] Add cotton wool compound N-[4-(2,4-dimethoxyphenyl)-5-oxo-4,5-2H[1,2]-dithiocyclopenta[4 ,3-b]pyrrol-6-yl]-3,5-bistrifluoromethylbenzamide and petroleum ether, heated or refluxed at 60°C for 0.5h; to N-[4-(2,4-dimethoxy phenyl)-5-oxo-4,5-2H[1,2]-dithiocyclopenta[4,3-b]pyrrol-6-yl]-3,5-bistrifluoromethane The benzamide is completely dissolved;
[0024] Slowly lower the temperature to 0°C, during the cooling process, fine crystal particles are continuously precipitated; filter to obtain N-[4-(2,4-dimethoxyphenyl)-5-oxo-4,5-2H[ 1,2]-Dithiocyclopenta[4,3-b]pyrrol-6-yl]-3,5-bistrifluoromethylbenzamide is yellow amorphous powder or fine needle crystal. ( 1 H NMR (CDCl 3 , ppm): 3.83(s, 3H), 3.87(s, 3H), 6.58(s, 1H), 6.63(m, 2H), 7.23(d, 1H), 8.11(s, 1H), 8.45(s, 2H), 8.64(s, 1H)).
Embodiment 2
[0026] Add cotton wool compound N-[4-(2,4-dimethoxyphenyl)-5-oxo-4,5-2H[1,2]-dithiocyclopenta[4 ,3-b]pyrrol-6-yl]-3,5-bistrifluoromethylbenzamide and a certain amount of petroleum ether, if there is still insoluble matter after heating at 60°C or refluxing for 1 hour, add hexane to The cotton wool-like substance was completely dissolved to obtain solution A;
[0027] The obtained solution A is subjected to vacuum rotary evaporation to remove the solvent (petroleum ether, hexane) contained therein, and fine crystal particles are continuously precipitated during the solvent evaporation process; rotary evaporation to dryness obtains N-[4-( 2,4-dimethoxyphenyl)-5-oxo-4,5-2H[1,2]-dithiocyclopenta[4,3-b]pyrrol-6-yl]-3 ,5-Bis trifluoromethyl benzamide yellow amorphous powder or fine needle crystals. ( 1 H NMR (CDCl 3 , ppm): 3.83(s,6H), 6.58(s,1H), 6.63(m,2H), 7.23(d,1H), 8.11(s, 1H), 8.45(s,2H), 8.64(s, 1H)).
Embodiment 3
[0029] Add cotton wool compound N-[4-(2,4-dimethoxyphenyl)-5-oxo-4,5-2H[1,2]-dithiocyclopenta[4 ,3-b]pyrrol-6-yl]-3,5-bistrifluoromethylbenzamide and a certain amount of benzene, heated or refluxed at 80°C for 1.5h, the cotton-like substance in the flask was partially dissolved, and the other part Although not dissolved, the crystal form has changed;
[0030] Cool slowly to 0°C, crystallize, filter off the solvent benzene, and the obtained crystals are yellow amorphous powder or fine needle crystals N-[4-(2,4-dimethoxyphenyl)-5-oxo- 4,5-2H[1,2]-dithiocyclopenta[4,3-b]pyrrol-6-yl]-3,5-bistrifluoromethylbenzamide. ( 1 H NMR (CDCl 3 , ppm): 3.84(s,3H), 3.87(s,3H), 6.58(s,1H), 6.63(m,2H), 7.23(d, 1H), 8.09(s,1H), 8.45(s, 2H), 8.64(s, 1H)).
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Abstract
The invention discloses a preparation technology for a crystal of a dithiole pyrrolones compound. N-[4-(2,4-dimethoxyphenyl)-5-oxo-4,5-2H[1,2]-dithiole[4,3-b]pyrrole-6-group]-3,5-bis-(trifluoromethyl)-benzamide is taken as the compound. The compound is heated in a non-polar organic solvent, thereby transforming a crystal form of the compound from flocculence form into amorphous powder or thin needle form. The preparation technology provided by the invention has the characteristics of mild condition and easiness in operation; compared with an original flocculence form structure, the prepared crystal compound in the amorphous powder or thin needle form has the advantages that the dispersibility of the compound can be enhanced and the medicinal effect can be promoted; the volume of the compound is obviously reduced by the crystal form in the amorphous powder or thin needle form, so that the compound is more simply and conveniently stored and transported; and the crystal compound in the amorphous powder or thin needle form prepared according to the preparation technology provided by the invention can be further used for preparing medicines for treating diseases such as leucopenia, hemodynamic disturbance, tumor, and the like.
Description
technical field [0001] The invention belongs to the field of chemistry, and relates to a process for preparing crystallization of a compound, specifically a process for preparing crystallization of a dithiolopyrrolone compound. The compound is N-[4-(2,4- Dimethoxyphenyl)-5-oxo-4,5-2H[1,2]-dithiocyclopenta[4,3-b]pyrrol-6-yl]-3,5-bis Trifluoromethylbenzamide. Background technique [0002] Reference Bioorganic & Medicinal Chemistry 15, 4601–4608 (2007) (Bin Li, Michael P. A. Lyle, Genhui Chen, et al), it is known that the compound N-[4-(2,4-dimethoxyphenyl) -5-oxo-4,5-2H[1,2]-dithiocyclopenta[4,3-b]pyrrol-6-yl]-3,5-bistrifluoromethylbenzamide The synthetic route of is as follows: [0003] [0004] The above-mentioned compound is a drug molecule with anti-leukopenia effect, which can promote the production of leukocytes in the human body, has obvious therapeutic effects on human tumor cells H460 and Lcc6, and helps prevent and treat HIV virus infection, which is produced b...
Claims
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