Method of refining verapamil hydrochloride

A technology of verapamil hydrochloride and its refining method, which is applied in the fields of carboxylic acid nitrile purification/separation, organic chemistry, etc.

Active Publication Date: 2011-04-27
TIANJIN CENT PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0031] There are other literature reports, according to the German patent 144052 report, using isopropanol, acetone single solvent or isopropanol and ethyl acetate recrystallization, can make vera hydrochloride The purity of pamil crude product improves, shows through our study, this method can make verapamil hydrochloride purity reach 98.4% indeed, fusing point 139-143, this method needs repeated recrystallization just can meet requirement, thereby has increased production cost

Method used

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  • Method of refining verapamil hydrochloride
  • Method of refining verapamil hydrochloride
  • Method of refining verapamil hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0049] The verapamil hydrochloride of 25 grams (HPLC is 96.5%) is added in the 250 milliliter round-bottomed reaction flasks that stirring and reflux condenser are equipped with, add 175 milliliters of acetone and 5 milliliters of water, after reflux is made to dissolve, add 1.2 grams of activated carbon, filtered, cooled to 15°C with stirring to precipitate crystals. Filtration, rinsing with acetone, and drying at 100°C gave 19.7 g of the product. HPLC showed that the purity was greater than 99.5% (area normalization method), and the melting point was 141.5-145°C.

Embodiment 2

[0051] The verapamil hydrochloride of 25 grams (HPLC is 96.5%) is added in the 250 milliliter round-bottom reaction flasks that stirring and reflux condenser are equipped with, add 125 milliliters of isopropanols and 5 milliliters of water, after reflux is made to dissolve, Add 1.2 g of activated carbon, filter, and cool to 15°C with stirring to precipitate crystals. Filtration, rinsing with isopropanol, and drying at 100°C yielded 21.2 g of the product. HPLC showed a purity greater than 99.5% (area normalization method), and a melting point of 141.5-145°C.

Embodiment 3

[0053] The verapamil hydrochloride of 50 kilograms (HPLC is 96.5%) is added in the reactor of 500 liters that stirring and reflux condenser are equipped with, add 350 liters of acetone and 5 liters of water, after heating and refluxing to make it dissolve, add 1.2 kilograms of gacs , filtered, and cooled to 15°C with stirring to precipitate crystals. Filter, wash with acetone, and dry at 100°C to obtain 44.5 kg of the product. HPLC shows that the purity is greater than 99.5% (area normalization method), and the melting point is 141.5-145°C.

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Abstract

The invention discloses a finishing method of alcaine verapamil, which is characterized by the following: dissolving rough product of alcaine verapamil in the fitful quantity of water or hot solution of isopropanol; adding active charcoal; filtering; cooling; evolving; recrystallizing; improving purity over 99.5% and fusing point to 141.5-145 deg.c.

Description

technical field [0001] The invention belongs to the field of organic chemistry and relates to a method for refining verapamil hydrochloride. technical background [0002] Phenylacetonitrile basic substitute formula (I): [0003] [0004] In the formula, R', R", R"', R 1 , R 2 and R 3 is a hydrogen atom, a halogen atom, a lower alkane, a lower alkoxyl, a lower alkylthio or an amino group, preferably a mono- or disubstituted lower alkane; R4 is a straight-chain or branched aliphatic hydrocarbon containing 1-6 carbon atoms, or Saturated or unsaturated aliphatic hydrocarbons containing 5-6 carbon atoms, R5 is a hydrogen atom or a lower alkane. [0005] The chemical name of verapamil hydrochloride is α-[3-[[2-(3,4-dimethoxyphenyl)ethyl]methylamino]propyl]-3,4-dimethoxy-α-iso Propylphenylacetonitrile hydrochloride [0006] [0007] This product is a calcium ion antagonist that can selectively dilate coronary arteries and increase coronary flow; it can inhibit myocardi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/34C07C255/43
Inventor 孟庆礼耿家志
Owner TIANJIN CENT PHARM CO LTD
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