Production method of levamlodipine besylate

A kind of technology of levamlodipine besylate and its production method, which is applied in the field of production of levamlodipine besylate, can solve the problem that there is no system for temperature adjustment and prevention of feed liquid oxidation, it is not suitable for refined filtration treatment, and the filter cannot avoid light and other problems, to achieve the effect of convenient filtration operation and assembly and cleaning, stable filtrate quality, and simple structure

Active Publication Date: 2009-07-15
HONGYI SCI & TECH CO LTD NANCHANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Levoamlodipine besylate is unstable in light, high temperature, high humidity and in the air, while the currently widely used filter cannot avoid light, has no temperature regulation and prevents the oxidation system of the feed liquid, and has low filtration efficiency and is not suitable for use in benzene Refining Filtration Treatment in the Production Process of Levoamlodipine Sulfonate

Method used

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  • Production method of levamlodipine besylate
  • Production method of levamlodipine besylate
  • Production method of levamlodipine besylate

Examples

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preparation example Construction

[0015] 1. Preparation of intermediate I crude product

[0016] Add 1kg (2.44mol) (±)-amlodipine and 84g (0.55mol) L-(+)-tartaric acid in a 10-liter reactor, then add 8 liters of DMF, stir at room temperature, react for 24 hours, suction filter, filter The cake was washed twice with DMF, 500ml each time, and the filter cake was vacuum-dried to prepare 440g of intermediate I crude product, with a yield of 36.9%.

[0017] 2. Refining of Intermediate I

[0018] Add 430g (0.89mol) of intermediate I crude product and DMF 1800ml into a 3-liter reactor, stir and react at 50°C for 5 hours, stop heating, cool, filter with suction, wash the filter cake with 500ml of DMF, and dry in vacuum to obtain Intermediate I. Sub-refined product 362g, yield 84.2%.

[0019] Add 360g (0.75mol) of the first refined product of intermediate I and 1500ml of DMF in a 3-liter reactor, stir and react at 50°C for 5 hours, stop heating, cool, filter with suction, wash the filter cake with 500ml of DMF, and d...

specific Embodiment approach

[0025] combined with figure 2Describe the specific implementation of the present invention using a special filter: a filter, including a filter top cover 1, ring groove filter plates 2 and 3, a filter barrel 4 and a filter bottom cover 5, a feed pipe 6, and an inert gas inlet pipe 7 , an inert gas outlet pipe 8, a cooling liquid outlet 9, a cooling liquid return pipe 10, and a temperature gauge 11 are respectively installed on the filter top cover 1, the filter top cover 1 is provided with an insulating layer 12 and an interlayer 13, and the filter barrel 4 is a cylindrical barrel Shaped, located at the bottom of the filter top cover 1, equipped with an insulating layer 27, an interlayer 28, an outer metal plate 15, a middle metal plate 16 and an inner metal plate 17, the filter bottom cover 5 is located at the bottom of the filter barrel 4, and is provided with an outlet Material pipe 18, coolant inlet 19, insulation layer 20 and interlayer 21, filter top cover 1 is hemisphe...

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Abstract

The invention takes N, N-dimethylformamide as a chiral auxiliary and separates amlodipine with tartaric acid resolution reagent to prepare l-amlodipine. In addition, benzene sulfonic acid and l-amlodipine alkali are directly salified and refined, filtered and dried via a special filter to produce levoamlodipine besylate. The upper part and the lower part of the special filter adopted by the invention are respectively provided with a hemispherical top cap and a hemispherical bottom cap, the middle part is provided with a lauter tank and ring groove filter plates are respectively arranged between the top cap and the lauter tank or the bottom cap and the lauter tank. A feed pipe, inlet and outlet of inert gases, an outlet of cooling fluid and a temperature meter are installed on the top cap of the filter; a discharge pipe and the outlet of cooling fluid are installed on the bottom cap. The filter is provided with an insulating layer and an interlayer, thus can control the temperature, avoid light, be filled with inert gases and protect the feed liquid and filtrate from oxidation, illumination and high temperature damage. The filtration efficiency is high, the effect is good and the structure is simple, the filter operation, disassembly, assembly and cleaning are convenient and the levoamlodipine besylate enjoys high synthesis and production yield and stable quality.

Description

technical field [0001] The present invention uses DMF as a chiral auxiliary agent to resolve (±)-amlodipine with L-(+)-tartaric acid resolution reagent to prepare levamlodipine, and directly forms a salt with benzenesulfonic acid and levamlodipine base. Special filtering device refines, filters and dries to produce levamlodipine besylate. Background technique [0002] The patent (CH1067055C, PCT / EP95 / 00847) of Pfizer Research and Development Company "Separation of its enantiomers from diastereomeric tartrates of arodipine" discloses the separation of its R-(+)- and the S-(-)-isomer, which involves the D - The DMSO solvate of the tartrate salt is precipitated in an organic solvent of dimethyl sulfoxide (DMSO) and the isomer mixture is reacted with L- or D-tartaric acid. [0003] "Resolution of Enantiomers of Amlodipine" (ZL 00102701.8) discloses a feasible resolution of the two (R)-(+)- and (S)-(-)-enantiomers of racemic amlodipine The method, the chiral reagent used for r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/90
Inventor 穆正义廖新华颜锋刘孝乐
Owner HONGYI SCI & TECH CO LTD NANCHANG
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