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S-nitrosocaptopril monohydrate crystal and preparation method thereof

A technology of monohydrate and hydrate, which is applied in the field of medicine, can solve the problem of difficulty in obtaining Cap-NO, and achieve the effect of good reproducibility, easy operation and good curative effect

Active Publication Date: 2018-05-08
福州光致科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Prior to this, we exclusively successfully synthesized the crystallization of solid Cap-NO, other laboratories around the world have used liquid Cap-NO for research, because solid Cap-NO is difficult to obtain

Method used

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  • S-nitrosocaptopril monohydrate crystal and preparation method thereof
  • S-nitrosocaptopril monohydrate crystal and preparation method thereof
  • S-nitrosocaptopril monohydrate crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Dissolve 10g of captopril and 3.5g of sodium nitrite in 35mL of 15wt% saline that has been cooled to 0°C, and add 20mg of EDTA-2Na·2H 2 0, stirring at 700 rpm for 1 h under ice bath conditions, then adding 24 wt% hydrochloric acid dropwise to adjust the pH to 4.0, so that a large amount of red Snopril monohydrate crystals are precipitated, suction filtered, and dried at room temperature (25 ° C), or Freeze-dried for 8 hours and stored in a refrigerator at 4°C or -20°C.

Embodiment 2

[0052] Dissolve 10g of captopril and 4.0g of sodium nitrite in 40mL of 15wt% saline that has been cooled to 0°C, stir at 1000rpm for 15min in an ice bath, then add 18wt% hydrochloric acid dropwise to adjust the pH to 4.0, making the red Si A large number of Nopril monohydrate crystals precipitated, filtered with suction, dried in an oven not exceeding 40°C for 1~8h, or dried in a vacuum oven at room temperature (25°C) for 10min~2h, and stored at 4°C or -20 ℃ in the refrigerator.

Embodiment 3

[0054] The powder X-ray diffraction (PXRD) collection of patterns of embodiment 1 Snopril monohydrate crystal is as figure 1 As shown, the PXRD characteristics are as follows:

[0055]

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Abstract

The invention reports a novel s-nitrosocaptopril monohydrate crystal form, a preparation method thereof as well as application of the crystal form to preparation of a medicinal composition for treating pulmonary hypertension, hypertension and congestive heart failure for the first time. The preparation method comprises the following steps: dissolving captopril, sodium nitrite and EDTA-2Na*2H2O into a salt solution of 15+ / -5 weight percent, performing reaction and adjusting the pH value of the solution so as to separate out s-nitrosocaptopril monohydrate crystals. The s-nitrosocaptopril monohydrate crystals can be stably stored under the environment of 4 DEG C for 12 months.

Description

technical field [0001] The invention belongs to the field of medicine, and relates to a novel Snopril monohydrate and a preparation method thereof; a pharmaceutical composition with the new Snopril crystal form as an active ingredient, and Snopril monohydrate and its preparation method. The application of the composition in the preparation of medicines for treating pulmonary hypertension, hypertension and congestive heart failure. Background technique [0002] Captopril, also known as Kaibotong (Capoten, Cap), is the first orally effective angiotensin-converting enzyme inhibitor (angiotensin-converting enzyme inhibitor, ACEI) (Jia Li. Angiotensin-converting enzyme inhibitor Advances in Physiological Sciences. Advances in Physiological Sciences, 1985, 16: 229-234). In 1977, Ondetti et al. completed the chemical synthesis and preliminary pharmacological experiments of Cap. In the following two decades, ACEI was widely used in the treatment of hypertension and heart failure i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/16A61P9/12A61P9/04A61P11/00
CPCC07B2200/13C07D207/16A61P9/04A61P9/12A61P11/00
Inventor 贾力周雨杨陈帆李飞杨林敏李书慧
Owner 福州光致科技有限公司
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