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

Eldecalcitol crystal form and preparation method thereof

A technology of idecalcidol and crystal form, applied in the field of compound preparation, can solve the problems of high production cost, high cost, high difficulty and the like, and achieve the effects of easy industrial scale-up, easy recovery and application, and easy operation

Inactive Publication Date: 2017-01-18
SHANGHAI HAOYUAN CHEMEXPRESS
View PDF2 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Due to the long and difficult synthetic route of Eldecalcitol, the production cost is high
With the development of modern separation technology, preparative liquid chromatography is widely used in the field of separation. In order to obtain as many high-purity products as possible, it is a good choice to purify crude idecalcitol by preparative liquid chromatography , but the idecalcitol obtained after separation is an amorphous solid. After research and comparison, it is found that the product stability of the amorphous solid is much lower than that of the solid product with a crystal form. At the same time, preparative liquid chromatography The cost of separation is also higher

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
  • Eldecalcitol crystal form and preparation method thereof
  • Eldecalcitol crystal form and preparation method thereof
  • Eldecalcitol crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Preparation of compound I crystal form A:

[0066] Mix 1 g of crude idecalcitol (purity 95%) and 10 mL of ethyl acetate in a round-bottomed flask, and heat in a water bath to an internal temperature of 35°C to 40°C under stirring until a transparent and uniform solution is formed. Stop heating, slowly cool down to room temperature, seal the round-bottom flask and place it at -18°C to freeze and crystallize. Take it out after 10 to 16 hours, filter, wash the filter cake with ethyl acetate at 0°C, collect the solid, and dry it in vacuum at room temperature to obtain 873 mg of white needle-like solid, with a yield of 87%.

[0067] Table 1 shows the X-ray powder diffraction data of Form A obtained in this example.

[0068] Table 1 X-ray powder diffraction data of crystal form A

[0069]

[0070]

Embodiment 2

[0072] Preparation of compound I crystal form B:

[0073] Mix 1 g of crude idecalcitol (purity 95%) and 10 mL of acetone in a round-bottomed flask, and heat in a water bath to an internal temperature of 35°C to 40°C under stirring until a transparent and uniform solution is formed. Stop heating, slowly cool down to room temperature, seal the round-bottom flask and place it at -18°C to freeze and crystallize. Take it out after 10 to 16 hours, filter, wash the filter cake with acetone at 0°C, collect the solid, and dry it under vacuum at room temperature to obtain 904 mg of white needle-like solid with a yield of 90%.

[0074] Table 2 X-ray powder diffraction data of crystal form B

[0075]

[0076]

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 relates to an Eldecalcitol crystal form and a preparation method thereof. The compound is used for treating osteoporosis. The method is simple and efficient to operate and is beneficial to industrial production; and the product has good crystal stability and high purity.

Description

[0001] Technical field: [0002] The invention relates to a preparation method of a compound, in particular to a crystal form of drug Eldecalcitol used for treating osteoporosis and a preparation method thereof. [0003] Background technique: [0004] Eldecalcitol is a drug developed by Chugai Pharmaceutical Co., Ltd. for the treatment of osteoporosis. It is a second-generation vitamin D3 analogue with a trade name of Currently only available in the Japanese market. [0005] [0006] The original manufacturer, Chugai Pharmaceutical Co., Ltd. only disclosed the synthesis and purification method of Eldecalcitol in patent WO1998000397, but the specific crystal form and detailed preparation method were not reported. Since then, journals, patents and technical documents related to the compound have not reported its crystal form and obtaining method. [0007] Because the synthetic route of Eldecalcitol (Eldecalcitol) is long and difficult, the production cost is high. With the...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07C401/00
CPCC07C401/00
Inventor 丁福斗张宪恕高强郑保富
Owner SHANGHAI HAOYUAN CHEMEXPRESS