Sodium bromide application experiment method

Abstract

The invention belongs to the technical field of valsartan intermediate synthetic product treatment, and particularly relates to a sodium bromide application experimental method. The method comprises the following steps: adding raw materials into a reaction kettle according to the weight ratio of sartan biphenyl, AIBN (azodiisobutyronitrile), sodium bromide, concentrated sulfuric acid, dichloromethane, drinking water and hydrogen peroxide, heating the reaction kettle, and dropwise adding hydrogen peroxide; after hydrogen peroxide is added, carrying out the heat preservation; when liquid becomes colorless and transparent, stopping heating, and carrying out the heat preservation; carrying out cooling, standing and layering; after liquid layering, taking out an organic layer and washing the organic layer; performing concentration after water washing, adding ethyl acetate into concentrated liquid, carrying out the crystallization, obtaining bromo-sartan biphenyl (4'-bromomethyl-2-cyanobiphenyl), and achieving the recycling of the bromine element, wherein the bromo-sartan biphenyl (4'-bromomethyl-2-cyanobiphenyl) obtained after recycling can be continuously used for valsartan intermediate N-[(2'-cyanobiphenyl-4-yl) methyl]-L-valine methyl ester hydrochloride, and therefore internal circulation of bromine is achieved, the cost is reduced, and environment-friendly emission is reduced.

Description

technical field [0001] The invention belongs to the technical field of valsartan intermediate synthesis product treatment, and in particular relates to a sodium bromide experimental method. Background technique [0002] Valsartan, chemical name: N-pentanoyl-N-[[2'-(1H-tetrazol-5-yl)[1,1'-biphenyl]-4-yl]methyl]-L- Valine has the advantages of long-lasting and stable blood pressure lowering effect, less side effects and can be used in combination with other sartan drugs. It is a widely used antihypertensive drug in clinical practice. The drug acts to block the type I (AT1) receptor of angiotensin II, selectively acts on the AT1 receptor subtype, blocks the combination of Ang II and AT1 receptor, and increases the plasma level of angiotensin II. Stimulate unblocked AT2 receptors and counteract the effect of AT1 receptors, so as to achieve the effect of dilating blood vessels and lowering blood pressure. [0003] When preparing valsartan, the intermediate N-[(2'-cyanobiphenyl-...

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Problems solved by technology

[0003] When preparing valsartan, the intermediate N-[(2'-cyanobiphenyl-4-yl)methyl]-L-valine methyl ester hydrochloride of valsartan should be prepared at first, through bromine Desartan biphenyl (4'-bromomethyl-2-cyanobiphenyl) and valine methyl ester react under the catalysis of sodium carbonate to generate N-[(2'-cyanobiphenyl-4-yl ) methyl]-L-valine methyl ester hydrochloride and sodium bromide, sodium bromide is not processed at present, direct discharge will pollute the environment and cause waste of bromine

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