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Drotaverine hydrochloride crystal form I and crystal form II and preparation method

A technology of drotaverine hydrochloride and crystal form, which is applied in the field of preparation of drotaverine hydrochloride, can solve problems such as unfavorable and stable storage, and achieve the effects of good purity and stability, good stability, and simple preparation method

Active Publication Date: 2014-03-26
ZHEJIANG APELOA KANGYU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

We found that the product obtained by crystallization in ethanol, the crystalline ethanol in the molecule is easy to exchange with the water molecule in the air, which is not conducive to stable storage

Method used

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  • Drotaverine hydrochloride crystal form I and crystal form II and preparation method
  • Drotaverine hydrochloride crystal form I and crystal form II and preparation method
  • Drotaverine hydrochloride crystal form I and crystal form II and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Preparation of drataverine hydrochloride crystal form I

[0046] Put 150mL of purified water, 22.5g of drotaverine hydrochloride, and 4.5mL of concentrated hydrochloric acid into a 250mL three-necked flask, and raise the temperature to 70°C. Most of the system will dissolve, and the undissolved part will turn pale yellow. After stirring for 30 minutes, remove the hot water bath, cool down to 30°C naturally, and filter with suction. The wet product was baked under reduced pressure in an oven at 50°C for 24 hours to obtain Form I with a yield of 86.4% and a water content of 4.0%. The HPLC purity is above 99.5%.

[0047] The H-NMR data of product are as follows:

[0048] 1H-NMR (500MHz, DMSO-d6, TMS) δ13.89 (s, 1H), δ7.59 (s, 1H), δ7.22 (d, J=1.5, 1H), δ7.10 (s, 1H ), δ6.92 (dd, J=8.3, 1.7, 1H), δ6.87 (d, J=8.3, 1H), δ4.53 (s, 2H), δ4.14~4.18 (q, J=6.9 , 2H), δ4.06~4.10 (q, J=6.9, 2H), δ3.98~4.02 (q, J=6.9, 2H), δ3.93~3.97 (q, J=6.8, 2H), δ3 .82 (t, J=7.9, 2H), δ2.97 ...

Embodiment 2

[0056] Preparation of drataverine hydrochloride crystal form II

[0057] Preparation of crystal form II of drotaverine hydrochloride: 150 mL of purified water, 22.5 g of drotaverine hydrochloride, and 4.5 mL of concentrated hydrochloric acid were put into a 250 mL three-necked flask, and the temperature was raised to 80°C. After the system was dissolved, cool it in a tap water bath, lower the temperature to 31°C, filter with suction, and dry the wet product in a 40°C oven under reduced pressure for 24 hours to obtain Form II, with a yield of 88.1% and a moisture content of 5.6%. HPLC purity is more than 99.5%, and nuclear magnetic detection data is with embodiment 1.

[0058] The sample prepared by this embodiment is subjected to X-ray powder diffraction detection (the detection instrument and scanning conditions are the same as in Example 1), and the detection results are shown in image 3 , image 3 The main characteristic peak parameters in are shown in the following tabl...

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Abstract

The invention discloses a drotaverine hydrochloride crystal form I, according to the crystal form I, the characteristic peaks are shown at the angles of 5.422 degrees, 6.699 degrees, 8.108 degrees, 10.067 degrees, 10.698 degrees, 12.093 degrees, 13.232 degrees, 14.513 degrees, 16.133 degrees, 22.183 degrees, 24.225 degrees and 24.766 degrees of the X-ray powder diffraction spectrogram expressed by the diffraction angle of (2 theta-0.2)-(2 theta+0.2) degrees. The invention further discloses a drotaverine hydrochloride crystal form II; according to the crystal form II, the characteristic peaks are shown at the angles of 3.955 degrees, 4.22 degrees, 6.364 degrees, 7.784 degrees, 8.307 degrees, 9.646 degrees, 11.628 degrees, 13.012 degrees, 13.233 degrees, 16.171 degrees, 17.379 degrees, 20.76 degrees and 23.262 degrees of the X-ray powder diffraction spectrogram expressed by the diffraction angle of (2 theta-0.2)-(2 theta+0.2) degrees. The invention further discloses a preparation of the crystal form I and the crystal form II. The crystal form I and the crystal form II disclosed by the invention are high in stability, and the preparation method is simple in process, and the practicability is high.

Description

technical field [0001] The invention relates to the technical field of preparation of drotaverine hydrochloride, in particular to crystal forms I and II of drotaverine hydrochloride and a preparation method. Background technique [0002] Papaverine (Papaverine) is an alkaloid isolated from opium. It has non-selective smooth muscle relaxation, weak central analgesic effect and local anesthetic effect. It is used to treat smooth muscle spasm in various situations, mainly including gastrointestinal spasm , biliary colic, ureteral colic, bronchospasm, angina and other disorders. [0003] Drotaverine is a derivative of papaverine. Its antispasmodic effect is stronger than that of papaverine and lasts longer, and it is non-addictive. It also has the effects of dilating coronary arteries and relaxing smooth muscles. Drotaverine hydrochloride has obvious antispasmodic, analgesic and symptom relieving effects on abdominal pain caused by peptic ulcer, biliary colic, acute pancreatiti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D217/20
CPCC07D217/20
Inventor 叶云生郭卫锋陈利平王哲清郭振荣
Owner ZHEJIANG APELOA KANGYU PHARMA
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