Unlock instant, AI-driven research and patent intelligence for your innovation.

Deslanoside crystal form and preparation method thereof

A technology of acetyl lanatoside crystals and deacetyl lanatosides, applied in the field of deacetyl lanatoside crystal forms and its preparation, achieving the effects of good stability, high reproducibility, and simple preparation process

Active Publication Date: 2021-02-19
上海联星医药科技有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is only one patent on the crystal form of deacetyllanatoside, and only one patent CN 107082794A was applied by Chengdu Beite Pharmaceutical Co., Ltd. in May 2017

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Deslanoside crystal form and preparation method thereof
  • Deslanoside crystal form and preparation method thereof
  • Deslanoside crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Example 1 Preparation of deacetyllanatoside crystal form III

[0059] Take 30g of deacetylated lanatoside, add it to a 5L three-necked flask, add 4500ml of anhydrous methanol, heat to reflux and stir for 30 minutes, wait until the solid is completely dissolved, then filter while hot, add the filtrate to a 10L rotary steamer, control the temperature of the water bath to 60 ±10°C, remove most of the methanol by distillation under reduced pressure, evaporate and crystallize until a large amount of white solid is precipitated, transfer the material in the evaporating flask to a 2L three-neck flask, and stir and crystallize the system at room temperature 20-30°C for 2 hours. After filtering, the filter cake was vacuum-dried at 85±3° C. for 4-6 hours to obtain 28 g of the target crystal form of lanatoside. HPLC purity ≥ 98.0%, simple impurity ≤ 1.0%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a deslanoside crystal form and a preparation method thereof, and provides a deslanoside crystal form III, which comprises the following characteristic peaks measured by a 2[theta] reflection angle of 5.9+ / -0.2 degrees, 8.3+ / -0.2 degrees, 12.5+ / -0.2 degrees, 14.7+ / -0.2 degrees, 17.5+ / -0.2 degrees, 17.9+ / -0.2 degrees, 20.8+ / -0.2 degrees and 22.7+ / -0.2 degrees in an X-ray diffraction pattern. According to the invention, the deslanoside crystal form is high in purity, good in stability, safe to store and suitable for current medicine preparation, research and development; and the preparation process is simple, safe, high in reproducibility and suitable for industrial production.

Description

technical field [0001] The invention relates to a crystal form of deacetyllanatoside and a preparation method thereof. Background technique [0002] The chemical name of deacetyllanatoside is: 3-[[O-β-D-glucopyranosyl-(1→4)-O-2,6-dideoxy-β-D-nucleo-hexapyranose Base-(1→4)-O-2,6-dideoxy-β-D-nucleo-hexapyranosyl-(1→4)-O-2,6-dideoxy-β-D-nucleo-hexyl Pyranosyl]oxo]-12,14-dihydroxy-cardio-20(22)-enolactone. Molecular formula: C 47 h 74 o 19 , Molecular weight: 943.08, the product is slightly soluble in methanol and ethanol, almost insoluble in water and chloroform. Calculated as dry product, including C 47 h 74 o 19 It should be 96.0% to 102.0%. The trade name of this product is Cedilan, which is mainly used for heart failure. Because of its fast action, it is suitable for patients with acute cardiac insufficiency or acute exacerbation of chronic cardiac insufficiency; it can also be used to control the ventricular rate of patients with atrial fibrillation and atrial fl...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07J19/00
CPCC07B2200/13C07H15/256C07H1/06
Inventor 陈小林占娅锋高鹏飞梁屹杨易可赵卫忠
Owner 上海联星医药科技有限公司