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

Amorphous substance of 17alpha-acetoxy-11beta-(4-N,N-dimethylaminophenyl)-19-norpregn-4,9-diene-3,20-diketone and preparation method thereof

A technology of dimethylaminophenyl and norpregnant, which is applied in the directions of steroids, organic chemistry, organic chemistry, etc., can solve the problems of poor thermal stability, not very good stability, low solubility of crystal form A, etc. problems, to achieve the effect of high product purity, scalable operation, and good solubility

Active Publication Date: 2013-05-15
江西迪赛诺制药有限公司 +1
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Crystal form B (isopropanol hemisolvate) is a solvate with poor thermal stability; crystal form A has low solubility and poor stability

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
  • Amorphous substance of 17alpha-acetoxy-11beta-(4-N,N-dimethylaminophenyl)-19-norpregn-4,9-diene-3,20-diketone and preparation method thereof
  • Amorphous substance of 17alpha-acetoxy-11beta-(4-N,N-dimethylaminophenyl)-19-norpregn-4,9-diene-3,20-diketone and preparation method thereof
  • Amorphous substance of 17alpha-acetoxy-11beta-(4-N,N-dimethylaminophenyl)-19-norpregn-4,9-diene-3,20-diketone and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 30mL of methanol to 5.0g of CDB-2914 (crystal form A) raw material, heat to 65°C, stir to dissolve the solid completely; after the raw material of CDB-2914 is completely dissolved, slowly add 100ml of water; Stir at 65°C for 4 hours; filter and dry under reduced pressure at 60°C for 12 hours to obtain 4.7g of product with a mass yield of 94% and an HPLC purity of 99.0%.

[0032] Get the amorphous sample of CDB-2914 prepared by the present embodiment, with 1.5460 angstroms wavelength α 1 , 1.54439 Angstroms wavelength α 2 The radiation source, the intensity ratio of α 1 / α 2 The powder X-ray diffraction (XRPD) spectrum that measures in the Dedye-Scherrer INEL CPS-120 equipment of 0.5,40kV voltage and 30mA current intensity is as figure 1 shown by figure 1 It can be seen that the prepared amorphous CDB-2914 does not contain identifiable diffraction peak shapes in the XRPD pattern.

Embodiment 2

[0034] Add 30mL of methanol to 5.0g of CDB-2914 (isopropanol hemisolvate) raw material, heat to 65°C, stir to dissolve the solid completely; after the CDB-2914 raw material is completely dissolved, slowly add 100ml of water; , continue to keep stirring at 65° C. for 4 hours; filter, and dry under reduced pressure at 60° C. for 12 hours to obtain 4.6 g of product with a mass yield of 92% and an HPLC purity of 99.1%.

[0035] The XRPD spectrum of the amorphous matter of CDB-2914 prepared in the present embodiment is as follows: figure 1 shown.

Embodiment 3

[0037] Add 30mL of methanol to 2.0g of CDB-2914 (crystal form A) raw material, heat to 50°C, stir to dissolve the solid completely; after the raw material of CDB-2914 is completely dissolved, slowly add 60ml of water; Stir at 50°C for 3 hours; filter and dry under reduced pressure at 60°C for 12 hours to obtain 1.8 g of product with a mass yield of 90% and an HPLC purity of 99.0%.

[0038] The XRPD spectrum of the amorphous matter of CDB-2914 prepared in the present embodiment is as follows: figure 1 shown.

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

Disclosed are an amorphous substance of 17a-acetoxy-11ß-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20- dione and a preparation method thereof. The said CDB-2914 amorphous substance generally has a powder X-ray diffraction pattern shown as figure 1. The method for preparing the product comprises: providing a solution of CDB-2914 raw material in an organic solvent, and then crystallizing in the presence of a reverse solvent at certain temperature to obtain CDB-2914 amorphous substance.

Description

technical field [0001] The present invention relates to a kind of 17α-acetoxy-11β-(4-N, N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione (CDB -2914) and its preparation method. Background technique [0002] CDB-2914 (Uliprisnil acetate), the molecular formula is C 30 h 37 NO 4 , molecular weight 475.634, CAS number 126784-99-4, chemical name: 17α-acetoxy-11β-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9 -diene-3,20-dione, its chemical structural formula is as follows: [0003] [0004] CDB-2914 is an emergency contraceptive drug jointly developed by the National Institute of Child Health and Human Development of the United States and HRA Pharmaceuticals of France. CDB-2914 (trade name ELLA) was approved in Europe in May 2009 and was first launched in the UK, Germany and France on October 1. On August 13, 2010, the US Food and Drug Administration (FDA) approved the marketing application of ELLA. [0005] In the patent US4954490, the compound CDB-2914 and its ...

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 Patents(China)
IPC IPC(8): C07J41/00
CPCC07J41/00C07J41/0083C07B2200/13
Inventor 安晓霞吕锋申淑匣
Owner 江西迪赛诺制药有限公司