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Low-cost method preparation for doxazosin mesylate controlled release tablets

A technology of doxazosin mesylate and controlled-release tablets, which is applied in the field of medicine, can solve the problems of high price and unfriendly environment, and achieve the effect of cost reduction

Inactive Publication Date: 2019-06-14
陕西卓力时代人力资源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is an important method for the synthesis of doxazosin mesylate controlled-release tablets, the key of which is to use the precious metal PtO 2 Catalytic imine reduction can also be reduced by Raney nickel, but the price of both (especially PtO 2 ) are high and are not environmentally friendly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: Preparation of sodium triacetoxyborohydride

[0018] Add 1000mL of toluene into a 10L three-necked reaction flask, and install mechanical stirring. Stirring was started, 38g of sodium borohydride was added, and an ice-water bath was added to the outside to cool down. 183 g of glacial acetic acid was added dropwise, and the mixture was stirred and reacted overnight. Filter, wash the filter cake with about 200 mL of toluene, filter dry, and place the obtained white solid in a vacuum oven to dry in vacuo to obtain the product for later use.

Embodiment 2

[0019] Example 2: Preparation of N-[(1R)-2-(4-methoxyphenyl)-1-methylethyl]-N-[(1R)-1-phenylethyl]amine hydrochloride

[0020] Put 1300mL of dichloromethane, 93.2g of R-α-phenylethylamine and 114.8g of p-methoxyphenylacetone into a 2000mL three-necked flask equipped with mechanical stirring, start stirring and add an ice-water bath to cool down, then add 42.0g of glacial acetic acid. Add 178.0 g of sodium triacetoxyborohydride in batches, after the addition is complete, stir the reaction at 10°C to 20°C, and track the reaction until complete by thin-layer chromatography. Add 700mL sodium hydroxide aqueous solution (containing about 56g of sodium hydroxide) to adjust the pH value to 9, separate the dichloromethane layer, then add 500mL hydrochloric acid aqueous solution to adjust the pH value to 1-2, separate the dichloromethane layer, add anhydrous Na2SO4 dried. The dichloromethane was recovered by distillation under reduced pressure to dryness, 1500 mL of acetone was added t...

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PUM

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Abstract

The invention relates to a preparation method of doxazosin mesylate controlled release tablets for treating urination disorder caused by prostatic hyperplasia, and belongs to the field of medicines. The invention provides a low-cost preparation method for doxazosin mesylate controlled release tablets.

Description

technical field [0001] The invention relates to a preparation method of doxazosin mesylate controlled-release tablets for treating urination disorder caused by benign prostatic hyperplasia, and belongs to the field of medicine. Background technique [0002] Doxazosin Mesylate Controlled-release Tablets were developed by the Central Research Institute of Japan's Yamanouchi Pharmaceutical Co., Ltd., developed by Yamanouchi Pharmaceutical Co, Ltd, approved by the FDA in July 1992, and listed for the first time in Japan in 1993. The trade name is "" Harnal" (Ha Le), for the treatment of urinary disorders caused by benign prostatic hyperplasia. It entered the Chinese market in 1996 and obtained administrative protection for pharmaceuticals on September 16, 1996. Among the currently published patents on the asymmetric synthesis of tamsulosin, EP0257787 introduces the use of chiral (R)-phenylethylamine as a raw material, through the reduction of imines induced by chirality, to obt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C217/58C07C303/40C07C311/37C07D405/12
Inventor 程淑清牛清玲
Owner 陕西卓力时代人力资源有限公司
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