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Taurohyodeoxycholic acid type II crystal and preparation method thereof

A technology of deoxycholic acid and suisulphonic acid, which is applied in the field of type II crystal of sulfodeoxycholic acid and its preparation, and in the field of compounds for treating cholesterol gallstones, and can solve problems such as not specifying the melting temperature of hyosodeoxycholic acid , to achieve the effect of ensuring uniform quality, good product fluidity and concentrated particle size distribution

Active Publication Date: 2013-08-28
SICHUAN KELUN PHARMA RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese patent CN1896091 discloses a method for preparing hyodeoxycholic acid, but does not indicate the melting temperature and infrared (IR) spectrum of hyodeoxycholic acid

Method used

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  • Taurohyodeoxycholic acid type II crystal and preparation method thereof
  • Taurohyodeoxycholic acid type II crystal and preparation method thereof
  • Taurohyodeoxycholic acid type II crystal and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Example 1: Preparation of Hysodeoxycholic Acid Type II Crystals

[0054] Step 1: Preparation of hysulfodeoxycholic acid

[0055] In a three-necked flask equipped with a thermometer, a stirrer and a dropping funnel, stir and mix 40.0g of hyodeoxycholic acid, 10.5g of triethylamine and 450mL of dioxane, cool the solution in an ice-water bath, and add dropwise at 10°C Ethyl chloroformate 11.5g, continue to stir and react for 30min after dropping, then raise the temperature to 15°C and stir for 20min, filter the reaction solution, remove the triethylamine salt, and use the filtrate for later use; dissolve 16.0g of taurine in 100mL of 1.5mol / L NaOH aqueous solution, drop into the above filtrate, after dropping, stir and react in an ice-water bath for 3h, filter the reaction solution, pass the filtrate through a chromatography column equipped with a 732-type strong acid ion exchange resin, and control the outflow rate to 300mL / h; collect the effluent , the solvent was evapor...

Embodiment 2

[0060] Example 2: Preparation of Hysodeoxycholic Acid Type II Crystals

[0061] Step 1: Preparation of hysulfodeoxycholic acid

[0062] In a three-necked flask equipped with a thermometer, a stirrer and a dropping funnel, stir and mix 35.0g of hyodeoxycholic acid, 12.5g of triethylamine and 400mL of dioxane, cool the solution in an ice-water bath, and add dropwise at 12°C Ethyl chloroformate 13.5g, continue to stir and react for 25min after dropping, then raise the temperature to 16°C and stir for 25min, filter the reaction solution, remove the triethylamine salt, and set aside the filtrate; dissolve 12.0g of taurine in 120mL of 1.5mol / L NaOH aqueous solution, drop into the above filtrate, after dropping, stir and react in an ice-water bath for 3.5h, filter the reaction solution, pass the filtrate through a chromatographic column equipped with a 732-type strong acid ion exchange resin, and control the outflow rate to 285mL / h; collect the outflow Liquid, the solvent is evapora...

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Abstract

The invention relates to a novel crystal of a compound, in particular to a type II crystal of a compound taurohyodeoxycholic acid for treating cholesterol gallstone, and a method for preparing the type II crystal. The novel crystal has high stability; and compared with a type I crystal, the type II crystal has the advantages of high crystallinity, concentrated particle size distribution, high product liquidity, surface finish and the like, better contributes to industrial production, can better ensure the quality uniformity of a preparation, and can ensure that a medicine is safe and effective.

Description

technical field [0001] The invention relates to a novel crystal of a compound, in particular to a type II crystal of a compound hyodeoxycholic acid used for treating cholesterol gallstones and a preparation method thereof. Background technique [0002] Hyodeoxycholic acid, the chemical name is 5β-cholanic acid-3α, 6α-dihydroxy-N-(2-sulfoethyl)-amide, and its chemical structure is as follows: [0003] [0004] Hyodeoxycholic acid (THDCA) is a combination of hyodeoxycholic acid (HDCA) and taurine, a natural cholic acid that only exists in small amounts in pig bile. Clinically, it is mainly used for the auxiliary treatment of cholesterol gallstones, bile indigestion and liver diseases. [0005] Example 3 of European Patent EP0582891 discloses the preparation method of hyodeoxycholic acid, and gives the melting point (MP) of hyodeoxycholic acid as 168°C-169°C. [0006] Chinese patent CN1896091 discloses a method for preparing hyodeoxycholic acid, but does not indicate the m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00
Inventor 崔德修
Owner SICHUAN KELUN PHARMA RES INST CO LTD