Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation and refining method of pomalidomide

A technology of polilidomide and its refining method, which is applied in the field of preparation and refining of polilidomide, can solve the problems of low yield, low purity of the final product, and complicated preparation and operation, and achieve high reaction yield and large implementation Value and socio-economic benefits, the effect of reasonable process conditions

Active Publication Date: 2014-01-08
HANGZHOU PIOPHARM PHARMA TECH
View PDF2 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to solve the shortcomings of existing polilidomide preparation operations that are complicated, the yield is low, and the purity of the final product is not high, the present invention provides a new preparation method, the preparation process is simple, the product purity and yield are high, and it is suitable for Industrial production

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
  • Preparation and refining method of pomalidomide
  • Preparation and refining method of pomalidomide
  • Preparation and refining method of pomalidomide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 3-Nitrophthalic anhydride (12.9g), α-aminoglutarimide hydrochloride (11.0g), acetonitrile (50ml), and acetic acid (10ml) were put into the reaction flask, heated and refluxed for 4 hours, Cool to room temperature, recover the solvent, add 50ml of water, precipitate a white solid, filter with suction, wash the solid with water, and dry under reduced pressure to obtain 16.7g, yield 83%, melting point > 200°C; 1 H NMR (DMSO- d6 ) δ: 11.17( s, 1H), 8.36 (d, J = 8.0 Hz, 1H), 8.25 (d, J = 8.0 Hz,1H), 8.10 (t, J = 7.5 Hz, 1H), 5.22 (dd, J = 13.0, 5.5 Hz, 1H ), 2.93-2.86 (m, 1H), 2.63-2.58 (m, 1H), 2.47-2.51 (m, 1H), 2.06-2.10 (m, 1H).

Embodiment 2

[0026] Put 3-nitrophthalic anhydride (12.9g), α-aminoglutarimide hydrochloride (11.0g), dioxane (50ml), and formic acid (20ml) into the reaction flask, heat up and reflux After 4 hours, cool to room temperature, recover the solvent, add 50ml of water, precipitate a white solid, filter with suction, wash the solid with water, and dry under reduced pressure to obtain 17.8g, yield 85%, melting point > 200°C;

Embodiment 3

[0028] Put 3-nitrophthalic anhydride (12.9g), α-aminoglutarimide hydrochloride (11.0g), toluene (60ml), p-toluenesulfonic acid (10g) into the reaction flask, and heat up to reflux After 8 hours, it was cooled to room temperature, the solvent was recovered, 150ml of water was added, a white solid was precipitated, filtered with suction, the solid was washed with water, and dried under reduced pressure to obtain 18.8g, yield 93.5%, melting point > 200°C.

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 method for preparing pomalidomide [3-amino-N-(2,6-dioxo-3-piperidyl)-phthalimide], which comprises steps of condensation reaction, catalytic hydrogenation, refining, and the like. The process route is novel, short in steps, high in reaction yield, good in product purity, and has great implementation value and social economic benefits.

Description

technical field [0001] The invention belongs to the field of pharmaceutical chemical synthesis, in particular to a method for preparing and refining polilidomide. Background technique [0002] Multiple myeloma (multiplemgeloma, MM) is a malignant B cell disease that is difficult to cure. The malignant cells in the bone marrow of patients continue to proliferate, causing normal cells to fail to function. It is caused by plasma cells in the bone marrow. It is a type of blood cancer. Affects middle-aged and elderly people. Pomalidomide is a new type of immunomodulator developed by Celgene Corporation of the United States. It was approved by the FDA in February 2013, and its trade name is Pomalyst. An immunomodulatory drug used to treat relapsed or refractory multiple myeloma, polilidomide destroys cancer cells by regulating the human immune system and inhibits the growth of cancer cells. [0003] The chemical name of polilidomide is 3-amino-N-(2,6-dioxo-3-piperidinyl)-phthali...

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): C07D401/04
CPCC07D401/04
Inventor 陈波盛荣尤丽敏
Owner HANGZHOU PIOPHARM PHARMA TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com