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

A kind of preparation method of pharmaceutical intermediate p-methylbenzhydryl alcohol

A technology of p-methylbenzophenone and p-methylbenzophenone, which is applied in the field of preparation of pharmaceutical intermediate p-methylbenzophenone, can solve the problem of incomplete conversion of benzophenone compounds, complicated operation process, Long reaction time and other problems, to achieve the effect of high product yield, high purity and short reaction time

Inactive Publication Date: 2011-11-30
NANTONG UNIVERSITY
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, the traditional synthesis method of benzophenone compounds is the reduction method of zinc powder, which has a long reaction time, incomplete conversion of benzophenone compounds, difficult separation, low product purity, and complicated operation process

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 pharmaceutical intermediate p-methylbenzhydryl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a three-necked reaction flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 40 mL of solvent, 19.6 g of p-methylbenzophenone, 13.3 g of sodium borohydride, and 0.8 g of a phase transfer catalyst. After the addition, start stirring, Control the reaction temperature at 20-40°C, stir vigorously for 4 hours, and stop the reaction after the liquid chromatography traces the reaction to be complete. Add 40mL of water to the reaction bottle, and a white precipitate will appear. Filter to obtain the crude product of p-methylbenzhydryl alcohol, the crude product After drying, ethanol is recrystallized to obtain refined p-methylbenzhydryl alcohol product. The yield of p-methylbenzhydryl alcohol reaches 97.59%, and the melting point is 50-54°C.

Embodiment 2

[0022] In a three-necked reaction flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 40 mL of solvent, 19.6 g of p-methylbenzophenone, 15.2 g of sodium borohydride, and 0.8 g of a phase transfer catalyst. After the addition, start stirring, Control the reaction temperature at 20-40°C, stir vigorously for 4 hours, and stop the reaction after the liquid chromatography traces the reaction to be complete. Add 40mL of water to the reaction bottle, and a white precipitate will appear. Filter to obtain the crude product of p-methylbenzhydryl alcohol, the crude product After drying, ethanol is recrystallized to obtain refined p-methylbenzhydryl alcohol product, the yield of p-methylbenzhydryl alcohol reaches 98.07%, and the melting point is 50-54°C.

Embodiment 3

[0024] In a three-necked reaction flask equipped with an electric stirrer, a reflux condenser and a thermometer, add 40 mL of solvent, 19.6 g of p-methylbenzophenone, 17.1 g of sodium borohydride, and 0.8 g of a phase transfer catalyst. After the addition, start stirring, Control the reaction temperature at 20-40°C, stir vigorously for 4 hours, and stop the reaction after the liquid chromatography traces the reaction to be complete. Add 40mL of water to the reaction bottle, and a white precipitate will appear. Filter to obtain the crude product of p-methylbenzhydryl alcohol, the crude product After drying, recrystallize ethanol to obtain refined p-methylbenzhydryl alcohol product. The yield of p-methylbenzhydryl alcohol reaches 97.38%, and the melting point is 50-54°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 preparation method of p-methylbenzophenone, a medical intermediate, which uses p-methylbenzophenone and sodium borohydride as raw materials and reacts in the presence of a phase transfer catalyst and a solvent to prepare p-methylbenzophenone Benzyl alcohol, the phase transfer catalyst is tetrabutylammonium bromide or cetyltrimethylammonium bromide or tetrapropylammonium bromide, and the solvent is ethanol or ethylene glycol. The separation and purification process of the method is simple, the reaction time is short, the product yield is high, and the product yield reaches more than 97%, and the obtained product has high purity, low energy consumption, little environmental pollution, and low cost. It is an ideal process for realizing industrial production. .

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate p-methylbenzhydryl alcohol. Background technique [0002] p-methylbenzhydryl alcohol, colorless needle-like crystals, melting point is 50-54°C. Mainly used in organic synthesis, pharmaceutical intermediates, and also a light absorber. [0003] Its chemical name is: p-methylbenzhydryl alcohol [0004] Molecular formula: C 14 h 14 O; molecular weight: 198.27 [0005] Molecular formula: [0006] [0007] Physical and chemical properties: Appearance is colorless needle-like crystals, melting point mp: 50-54°C, boiling point bp: 335°C. [0008] At present, the traditional synthesis method of benzophenone compounds is the zinc powder reduction method. This method has a long reaction time, incomplete conversion of benzophenone compounds, difficult separation, low product purity and complicated operation process. According to literature reports, the synthesis methods of be...

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): C07C33/24C07C29/143
Inventor 李建华王树清华平朱国华苏广均
Owner NANTONG UNIVERSITY
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