92075-58-6Relevant academic research and scientific papers
Preparation method of arotinolol hydrochloride
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, (2021/07/09)
The invention relates to the technical field of medicines, particularly provides a preparation method of arotinolol hydrochloride, and relates to the technical field of medicines. The preparation method of the arotinolol hydrochloride, provided by the invention, comprises the following steps: (1) enabling tetrahydrofuran, 2-formamide-5-(2-sulfydryl-1, 3-thiazole-4-yl)-thiophene, water, sodium bicarbonate and epoxy chloropropane to react to generate an intermediate product C181101170-I03; (2) carrying out a reaction on absolute ethyl alcohol, C181101170-I03 and tert-butylamine, so as to obtain an intermediate product C181101170-I02; (3) subjecting methanol, ethyl acetate, C181101170-I02 and concentrated hydrochloric acid to a reaction, and obtaining an arotinolol hydrochloride crude product; and (4) treating the arotinolol hydrochloride crude product with DMSO and acetone to obtain arotinolol hydrochloride. The product arotinolol hydrochloride obtained by the method is high in yield, high in purity and small in impurity, the purity of the product can be well controlled, and the method is suitable for industrial production.
Preparation and evaluation of a triazole-bridged bis(β-cyclodextrin)–bonded chiral stationary phase for HPLC
Shuang, Yazhou,Liao, Yuqin,Wang, Hui,Wang, Yuanxing,Li, Laisheng
, p. 168 - 184 (2019/11/25)
A triazole-bridged bis(β-cyclodextrin) was synthesized via a high-yield Click Chemistry reaction between 6-azido-β-cyclodextrin and 6-propynylamino-β-cyclodextrin, and then it was bonded onto ordered silica gel SBA-15 to obtain a novel triazole-bridged bis (β-cyclodextrin)–bonded chiral stationary phase (TBCDP). The structures of the bridged cyclodextrin and TBCDP were characterized by the infrared spectroscopy, mass spectrometry, elemental analysis, and thermogravimetric analysis. The chiral performance of TBCDP was evaluated by using chiral pesticides and drugs as probes including triazoles, flavanones, dansyl amino acids and β-blockers. Some effects of the composition in mobile phase and pH value on the enantioseparations were investigated in different modes. The nine triazoles, eight flavanones, and eight dansyl amino acids were successfully resolved on TBCDP under the reversed phase with the resolutions of hexaconazole, 2′-hydroxyflavanone, and dansyl-DL-tyrosine, which were 2.49, 5.40, and 3.25 within 30 minutes, respectively. The ten β-blockers were also separated under the polar organic mode with the resolution of arotinolol reached 1.71. Some related separation mechanisms were discussed preliminary. Compared with the native cyclodextrin stationary phase (CDSP), TBCDP has higher enantioselectivity to separate more analytes, which benefited from the synergistic inclusion ability of the two adjacent cavities and bridging linker of TBCDP, thereby enabling it a promising prospect in chiral drugs and food analysis.
Preparation process for arotinolol hydrochloride with high purity
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, (2018/03/26)
The invention discloses a preparation process for arotinolol hydrochloride with high purity. The preparation process comprises the following steps: pouring an acid-binding agent into an alcohol-watercompounded solvent, adding a compound namely 5-(2-sulfhydryl-4-thiazole)-2-thiophenecarboxamide, then adding epichlorohydrin, carrying out a reaction at a room temperature, and carrying out filteringand drying so as to obtain an intermediate III; pouring tert-butylamine into anhydrous ethanol, adding the intermediate III, carrying out a micro-reflux reaction, carrying out concentration, adding purified water, carrying out dissolving under heating, carrying out cooling, adjusting the pH value of an obtained solution to be acidic, carrying out washing with an organic solvent, adding ethanol into an aqueous layer, carrying out dissolving under heating, and carrying out cooling crystallization, and carrying out filtering so as to obtain a crude product; and pouring the crude product into an alcohol-water compounded solvent, carrying out dissolving under heating, and carrying out cooling crystallization, filtering and drying so as to obtain the arotinolol hydrochloride with high purity. The preparation process provided by the invention can effectively remove impurities from arotinolol hydrochloride, can reach a purity of 99.95% or above, and has simple operation and high yield.
Refinement method of arotinolol hydrochloride
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Paragraph 0018; 0020; 0022; 0024, (2018/02/04)
The invention relates to a refinement method of arotinolol hydrochloride and belongs to the field of chemical medicines. The refinement method is characterized in that crude arotinolol hydrochloride is added to a system containing ethyl acetate, methanol and pure water, subjected to an alkali recovery operation under a weak alkaline condition, then pulped and purified, and free alkaline arotinolol with higher purity is obtained; arotinolol forms salt in an alcoholic solution, and refined arotinolol hydrochloride is obtained. The method is simple to operate, the yield is relatively high, and industrial production is facilitated.
THERAPY FOR COMPLICATIONS OF DIABETES
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, (2009/07/02)
A method for enhancing glycemic control and/or insulin sensitivity in a human subject having diabetic nephropathy and/or metabolic syndrome comprises administering to the subject a selective endothelin A (ETA) receptor antagonist in a glycemic control and/or insulin sensitivity enhancing effective amount. A method for treating a complex of comorbidities in an elderly diabetic human subject comprises administering to the subject a selective ETA receptor antagonist in combination or as adjunctive therapy with at least one additional agent that is (i) other than a selective ETA receptor antagonist and (ii) effective in treatment of diabetes and/or at least one of said comorbidities other than hypertension. A therapeutic combination useful in such a method comprises a selective ETA receptor antagonist and at least one antidiabetic, anti-obesity or antidyslipidemic agent other than a selective ETA receptor antagonist.
ANTIHYPERTENSIVE THERAPY
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, (2009/09/08)
A new use of darusentan is provided in preparation of a pharmaceutical composition for lowering blood pressure in a patient exhibiting resistance to a baseline antihypertensive therapy with one or more drugs. The composition comprises darusentan in an amount providing a therapeutically effective daily dose; wherein (a) the composition is orally deliverable and/or (b) the daily dose of darusentan is effective to provide a reduction of at least about 3 mmHg in one or more blood pressure parameters selected from trough sitting systolic, trough sitting diastolic, 24-hour ambulatory systolic, 24-hour ambulatory diastolic, maximum diurnal systolic and maximum diurnal diastolic blood pressures. Further provided is a new use of darusentan in preparation of a pharmaceutical composition for lowering blood pressure in a patient exhibiting resistance to a baseline antihypertensive therapy, wherein the composition is administered adjunctively with at least one diuretic and at least one antihypertensive drug selected from ACE inhibitors, angiotensin II receptor blockers, beta-adrenergic receptor blockers and calcium channel blockers.
THIAZOLE DERIVATIVES
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, (2008/06/13)
This invention relates to thiazole derivatives of the formula (I): EQU1 wherein R 1 and R 2 are each hydrogen, lower alkyl, cycloalkyl, optionally substituted aryl or optionally substituted heteroaromatic rings containing oxygen, sulfur, nitrogen or combi
