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Preparation method of (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex

A technology of amlodipine and -dmso-d6, which is applied in the preparation of organic compounds, separation/purification of carboxylic acid compounds, preparation of carboxylate, etc., can solve the problem of low yield

Active Publication Date: 2014-11-19
SHIHUIDA PHARMA GRP (JILIN) LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Levoamlodipine is an important raw material for preparing antihypertensive drug preparations, and the patent literature of "Separation of Amlodipine Enantiomers" (00102701.8) discloses the use of D-tartaric acid and hexadeuteriodimethylsulfoxide (DMSO- d6) resolution amlodipine can obtain the method of high-purity levoamlodipine, but the yield of this method is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1 first 30g racemate amlodipine is dissolved in 137.4g DMSO-d6, makes the DMSO-d6 solution of amlodipine, with 2.748g D-tartaric acid under stirring condition (stirring speed 50rad / min) with Add it into the DMSO-d6 solution of amlodipine at a rate of 1ml / min, heat it to 35°C at the same time, keep stirring for 3 hours and then cool it down to room temperature naturally, at this time (S)-(-)-amlodipine-semi-D- The tartaric acid-mono-DMSO-d6 complex was precipitated and separated out, and the precipitate was filtered, washed, and dried to obtain a crude product of (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex. Add the crude complex to 500ml of ethyl acetate, heat to 40°C to dissolve it completely, cool down to room temperature at a rate of 2°C per hour to crystallize, add an appropriate amount of acetone to wash the precipitate, and dry it in vacuum at 50°C to obtain recrystallization The final (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6...

Embodiment 2

[0015] Embodiment 2 First 30g racemic amlodipine is dissolved in 137.4g DMSO-d6, makes the DMSO-d6 solution of amlodipine, with 2.748g D-tartaric acid under stirring condition (stirring speed 100rad / min) with Add it into the DMSO-d6 solution of amlodipine at a speed of 1ml / min, heat to 40°C at the same time, keep stirring for 2 hours and then cool to room temperature naturally, at this time (S)-(-)-amlodipine-semi-D- The tartaric acid-mono-DMSO-d6 complex was precipitated and separated out, and the precipitate was filtered, washed, and dried to obtain a crude product of (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex. Add the crude complex to 500ml of ethyl acetate, heat to 40°C to dissolve it completely, cool down to room temperature at a rate of 2°C per hour to crystallize, add an appropriate amount of acetone to wash the precipitate, and dry it in vacuum at 50°C to obtain recrystallization The final (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex w...

Embodiment 3

[0016] Embodiment 3 First 30g racemic amlodipine is dissolved in 137.4g DMSO-d6, makes the DMSO-d6 solution of amlodipine, with 2.748g D-tartaric acid under stirring condition (stirring speed 50rad / min) with Add it into the DMSO-d6 solution of amlodipine at a rate of 1ml / min, heat to 45°C at the same time, keep stirring for 3 hours and then cool to room temperature naturally, at this time (S)-(-)-amlodipine-semi-D- The tartaric acid-mono-DMSO-d6 complex was precipitated and separated out, and the precipitate was filtered, washed, and dried to obtain a crude product of (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex. Add the crude complex to 500ml of ethyl acetate, heat to 40°C to dissolve it completely, cool down to room temperature at a rate of 2°C per hour to crystallize, add an appropriate amount of acetone to wash the precipitate, and dry it in vacuum at 50°C to obtain recrystallization The final (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex was...

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Abstract

The invention provides a preparation method of a (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex, which comprises the following steps: resolving racemate amlodipine, recrystallizing a complex crude product, and finally obtaining the (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex. The method can obviously enhance the yield of the (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex.

Description

technical field [0001] The invention belongs to the technical field of medicine, and specifically relates to a method for preparing (S)-(-)-amlodipine-semi-D-tartaric acid-mono-DMSO-d6 complex from racemic amlodipine. Background technique [0002] (S)-(-)-amlodipine-half-D-tartaric acid-mono-DMSO-d6 complex is an intermediate for the preparation of (S)-(-)-amlodipine, the yield and purity of the intermediate It directly affects the yield and purity of (S)-(-)-amlodipine prepared at last. [0003] Levoamlodipine is an important raw material for preparing antihypertensive drug preparations, and the patent literature of "Separation of Amlodipine Enantiomers" (00102701.8) discloses the use of D-tartaric acid and hexadeuteriodimethylsulfoxide (DMSO- d6) The method for resolving amlodipine to obtain high-purity levamlodipine, but the yield of this method is not high. Contents of the invention [0004] The present invention provides a kind of preparation method of (S)-(-)-amlod...

Claims

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Application Information

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IPC IPC(8): C07D211/90C07C51/41C07C51/43C07C59/255
CPCC07C51/412C07C51/43C07D211/90C07C59/255
Inventor 何彧李环薛传校
Owner SHIHUIDA PHARMA GRP (JILIN) LTD
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