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

A kind of preparation method of tadala amorphous form I

A technology of tadalafil and crystal form, which is applied in the field of chemical pharmacy, can solve the problems of high cost of recovery and application of mixed solvents, high requirements for labor protection of workshop workers, and difficult removal of acetic acid residues, so as to be beneficial to energy saving, emission reduction and environmental protection , The effect of low labor protection requirements and low cost in the workshop

Active Publication Date: 2020-09-04
SHANDONG MINGREN FURUIDA PHARMA
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that acetic acid severely corrodes the equipment, and the residue of acetic acid is not easy to remove, which affects product quality
In addition, the cost of recovery and application of mixed solvents is high, the pressure on environmental protection is high, and the requirements for labor protection of workshop workers are high.

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
  • A kind of preparation method of tadala amorphous form I

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0030] The preparation of tadalafil crude product is according to literature:

[0031] Yao Shaobo, Cai Mingde, Lu Xiaoyi, etc. Synthesis of Tadalafil, Fine Chemical Intermediates[J].2010,40(6):39-42.

[0032] 520 g of crude tadalafil was prepared, and the product purity (HPLC normalization method, the same below): 98.99%.

Embodiment 1

[0034] Under nitrogen protection, add 150mL of acetonitrile aqueous solution (10:1 by volume), 10.0g of crude tadalafil, and 0.05g of SDS to the three-neck flask successively, stir for 10min, heat to 65-70°C, the system is dissolved, and then depressurize About 30mL of solvent was distilled off. After the evaporation was complete, the temperature of the system was lowered to -5-0°C, crystallized for 1 hour, filtered, washed with purified water at 40-50°C, and the filter cake was dried under reduced pressure at 50-60°C to obtain tadalafil ( Crystal form I) 9.16g, yield 91.6%.

Embodiment 2

[0036] Under the protection of nitrogen, 100mL of acetonitrile aqueous solution (volume ratio 6:1), 10g of crude tadalafil, and 0.25g of SDS were successively added to the three-neck flask, stirred for 10min, heated to 70-80°C, the system was dissolved, and then evaporated under reduced pressure. About 33mL of solvent was removed, after evaporation was complete, the system was cooled to 0-5°C, crystallized for 3 hours, washed with purified water at 40-50°C, filtered, and the filter cake was dried under reduced pressure at 50-60°C to obtain tadalafil (crystalline form Ⅰ) 9.29g, yield 92.9%.

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 provides a preparation method of Tadalafil crystal form I. The preparation method comprises the following steps: dissolving a Tadalafil crude product and SDS (Sodium Dodecyl Sulphate) inacetonitrile water together, and evaporating, decreasing temperature and crystallizing to prepare the Tadalafil crystal form I. According to the preparation method of the Tadalafil crystal form I, the using amount of a solvent is improved from existing 50 to 80 times to 8 to 20 times by introducing the SDS, so that the using amount of an organic solvent is greatly reduced. Moreover, the method provided by the invention is easy to operate, high in yield, short in production period and lower in cost, and is more suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical pharmacy, and in particular relates to a preparation method of tadalamorph I. Background technique [0002] Tadalafil, trade name Cialis, chemical name (6a,12aR)-6-(1,3-benzodioxol-5-yl)-2-methyl-2 ,3,7,12,12a-Hexahydropyrazino[1′,2′-1,6]indole-1,4-dione is a second-generation phosphoric acid jointly developed by Aikes and Eli Lilly and Company Diesterase inhibitors (PDE5 inhibitors), which competitively inhibit the combination of cGMP and PDE5, thereby inactivating PDE5, reducing the hydrolysis of cGMP, and increasing the concentration of cGMP to enhance erectile function. The chemical structural formula of tadalafil is as follows: [0003] [0004] In 2003, the FDA approved its marketing in the United States, and its indication was male erectile dysfunction (ED); in 2005, it was approved for domestic marketing in China. The recommended oral dose of tadalafil is 10-20mg / d. Compared with si...

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): C07D471/14
CPCC07B2200/13C07D471/14
Inventor 吴世德杨传伟贾美春刘文涛李新志刘杰江玉娟王莉姚玉娜
Owner SHANDONG MINGREN FURUIDA PHARMA
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