Crystallizing method for preparing high-purity 4-bromomethyl-2-cyanobiphenyl

A technique for bromosartan biphenyl and crude sartan biphenyl, which is applied in the field of crystallization for preparing high-purity bromosartan biphenyl, and can solve the problem that the mass yield is not more than 75%, the purity is lower than 99%, and it is difficult to Obtaining yield and other issues to achieve the effect of reducing side reactions, high yield per pass, and uniform particle size distribution
CN103626677BActive Publication Date: 2015-07-15TIANJIN UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
TIANJIN UNIV
Publication Date
2015-07-15

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Abstract

The invention relates to a crystallizing method for preparing high-purity 4-bromomethyl-2-cyanobiphenyl. The crystallizing method comprises the following steps: adding a 4-bromomethyl-2-cyanobiphenyl crude product in a solvent according to 0.4-0.65 g / mL of the solution concentration, stirring and dissolving the crude product at 40-60 DEG C, carrying out cooling and sterilization, reducing the temperature to 5-20 DEG C, keeping the temperature constant for 30-60 minutes, adding an elution agent to carry out solvent dilution crystallization, filtering, washing and drying the crystal mush to obtain the 4-bromomethyl-2-cyanobiphenyl product. The product color is purely white; the high performance liquid chromatography purity is up to 99.5%; the crystal granularity is large, the main granularity is about 100 microns, and the granularity distribution is uniform. During crystallization, the once through yield is high, so that the post treatment cost is saved. The method can provide the high-quality raw material for follow-up synthesis of sartan drug products, reduces unnecessary side reaction during the synthetic process, improves the quality indexes such as impurity and yield of the sartan drug products, and has good industrial application prospect.
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Description

technical field

[0001] The invention belongs to the technical field of chemical engineering crystallization, in particular to a crystallization method for preparing high-purity bromosartan biphenyl. Background technique

[0002] Hypertension is a major risk factor for cardiovascular and renal vascular diseases. Currently, there are many types of antihypertensive drugs clinically, but most of them have side effects other than the antihypertensive effect. Sartan drugs, also known as angiotensin II (Ang II) receptor (AT1) antagonists, can effectively intervene in the renin-angiotensin-aldosterone system (RAAS), and are important drugs for the treatment of hypertension. Sartan drugs can be used to treat all kinds of mild and moderate hypertension, and their antihypertensive effect is not inferior to that of various existing antihypertensive drugs, especially for patients who are intolerant to AngⅡ receptor blockers. A new generation of oral potent antihypertensive drugs with gr...

Claims

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