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

Preparation method of cyclohexyl acetone

A technology of cyclohexylacetone and acetone, which is applied in the field of preparation of cyclohexylacetone, can solve problems such as inability to carry out large-scale production, and achieve the effects of increased yield, simple post-treatment, and mild reaction conditions

Active Publication Date: 2021-05-28
枣庄市润安制药新材料有限公司
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The main purpose of the present invention is to provide a kind of preparation method of cyclohexyl acetone, to solve the problem that prior art cannot carry out large-scale 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 method of cyclohexyl acetone
  • Preparation method of cyclohexyl acetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] To acetone (580.80 g, 10 mol) in acetic acid (1 L) was added manganese acetate (4.90 g, 0.02 mol), cobalt acetate (0.89 g, 5 mmol) and cyclohexene (82.15 g, 1 mol) in sequence. The temperature was raised to 65°C, and oxygen was introduced into the reaction liquid. After the gas phase detection reaction was completed, it was lowered to room temperature. The insoluble matter was removed by filtration, and the filtrate was distilled under reduced pressure to obtain the product (85.54 g, 61%). The evaporated acetone and acetic acid can be recycled and reused. 1 H NMR (CDCl 3 , 400MHz) δ2.28(d, 2H, J=6.8Hz); 2.11(s, 3H); 1.85-1.75(m, 1H); 1.69-1.61(m, 4H); 1.30-1.08(m, 4H) ; 0.94-0.85 (m, 2H).

Embodiment 2

[0044] To a solution of acetone (58.08 g, 1 mol) in acetic acid (100 mL), nickel acetylacetonate (0.26 g, 1 mmol), cobalt acetate (0.09 g, 0.5 mmol) and cyclohexene (8.22 g, 0.1 mol) were added sequentially. The temperature was raised to 65°C, and oxygen was introduced into the reaction liquid. After the gas phase detection reaction was completed, the product (5.05 g, 36%) was obtained according to the post-treatment method of Example 1.

Embodiment 3

[0046] To acetone (58.08 g, 1 mol) in acetic acid (100 mL) was added manganese acetate (0.49 g, 2 mmol), cobalt acetate (0.09 g, 0.5 mmol) and cyclohexene (8.22 g, 0.1 mol) in sequence. The temperature was raised to 65° C., and air was introduced into the reaction liquid. After the gas phase detection reaction was completed, the product (7.43g, 53%) was obtained according to the post-processing method of Example 1.

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 cyclohexyl acetone, and particularly relates to the preparation method of cyclohexyl acetone by reacting a first catalyst, a second catalyst, cyclohexene and acetone with a mixed gas containing nitrogen and oxygen in acetic acid. The method disclosed by the invention is simple to operate, mild in reaction condition, less in generated solid waste, simple in post-treatment, recyclable in solvent and suitable for industrial production, and a reaction reagent with relatively high toxicity is avoided.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular, the invention provides a preparation method of cyclohexylacetone. Background technique [0002] Cyclohexylacetone is an important medicine and dye intermediate. In recent ten years, there have been many reports on the synthesis of this compound abroad. The main method is to use acetone and cyclohexene as raw materials to obtain it through free radical addition. [0003] In the literature report on the preparation of cyclohexylacetone, Shiraishi et al. (Org. Lett. 2008, 10, 3117-3120) used water as a solvent to generate acetone radicals by light to react with cyclohexene to obtain the target product. The reaction conditions have a low yield and high light intensity, which requires strict equipment. [0004] Linker et al. (Tetrahedron 1995, 51, 9917-9926) prepared cyclohexylacetone by oxidation of trivalent manganese to generate acetone radical. Although the yield of this method h...

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): C07C45/69C07C49/11
CPCC07C45/69C07C2601/14C07C49/11
Inventor 张奉志杨修东陈善任徐欣葛均官郭鹏张美堂
Owner 枣庄市润安制药新材料有限公司
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