Acetyl ferrocene synthesis method

A technology for the synthesis of acetyl ferrocene, which is applied in the fields of chemical instruments and methods, metallocenes, organic chemistry, etc., can solve the problems of difficult post-processing, harsh reaction conditions, and low yield, and achieve easy temperature control and synthesis The effect of mild reaction conditions and high production yield

Inactive Publication Date: 2017-12-19
苏州天允金属材料有限公司
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods have harsh reaction conditions at low temperatures, and have the disadvantages of low yield and difficult post-processing

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] One, the synthetic method of acetyl ferrocene

[0022] 1. Mix acetic anhydride and phosphoric acid and stir at room temperature for 15 minutes;

[0023] 2. Add ferrocene solid and heat up to 40°C for 1 hour;

[0024] 3. Heat up to 50°C and react until the ferrocene reaction is complete;

[0025] 4. Quickly pour the completed reaction solution into crushed ice, adjust the pH to 6-7 with solid sodium bicarbonate, and filter to obtain the crude acetylferrocene;

[0026] 5. Obtain pure acetyl ferrocene by recrystallization from petroleum ether.

[0027] In this embodiment, acetic anhydride:phosphoric acid:ferrocene solid=3:1:0.5.

[0028] Tested by elemental analysis, it was confirmed that the product was acetyl ferrocene. The yield is above 95%.

[0029] The synthesis reaction conditions of acetyl ferrocene are mild, the temperature is easy to control, and the preparation yield is high.

[0030] Two, the synthetic method of α-bromo-acetyl ferrocene

[0031] 1. Mix a...

Embodiment 2

[0039] One, the synthetic method of acetyl ferrocene

[0040] 1. Mix acetic anhydride and phosphoric acid and stir at room temperature for 10 minutes;

[0041] 2. Add ferrocene solid, heat up to 35°C for 1 hour;

[0042] 3. Heat up to 50°C and react until the ferrocene reaction is complete;

[0043] 4. Quickly pour the completed reaction solution into crushed ice, adjust the pH to 6-7 with solid sodium bicarbonate, and filter to obtain the crude acetylferrocene;

[0044] 5. Obtain pure acetyl ferrocene by recrystallization from petroleum ether.

[0045] In this example, acetic anhydride:phosphoric acid:ferrocene solid=3:1:0.45.

[0046] Tested by elemental analysis, it was confirmed that the product was acetyl ferrocene. Yield 94.7%.

[0047] The synthesis reaction conditions of acetyl ferrocene are mild, the temperature is easy to control, and the preparation yield is high.

[0048] Two, the synthetic method of α-bromo-acetyl ferrocene

[0049] 1. Mix acetylferrocene, ...

Embodiment 3

[0057] One, the synthetic method of acetyl ferrocene

[0058] 1. Mix acetic anhydride and phosphoric acid and stir at room temperature for 15 minutes;

[0059] 2. Add ferrocene solid and heat up to 40°C for 1 hour;

[0060] 3. Heat up to 50°C and react until the ferrocene reaction is complete;

[0061] 4. Quickly pour the completed reaction solution into crushed ice, adjust the pH to 6-7 with solid sodium bicarbonate, and filter to obtain the crude acetylferrocene;

[0062] 5. Obtain pure acetyl ferrocene by recrystallization from petroleum ether.

[0063] In this embodiment, acetic anhydride:phosphoric acid:ferrocene solid=2.8:1:0.5.

[0064] Tested by elemental analysis, it was confirmed that the product was acetyl ferrocene. Yield 93.8%.

[0065] The synthesis reaction conditions of acetyl ferrocene are mild, the temperature is easy to control, and the preparation yield is high.

[0066] Two, the synthetic method of α-bromo-acetyl ferrocene

[0067] 1. Mix acetylferr...

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 an acetyl ferrocene synthesis method, which comprises: (1) mixing acetic anhydride and phosphoric acid, and stirring for 10-15 min at a room temperature; (2) adding a ferrocene solid, heating to a temperature of 35-40 DEG C, and carrying out thermal insulation; (3) heating to a temperature of 45-50 DEG C, and carrying out a reaction until the ferrocene completely reacts; (4) rapidly pouring the reaction solution into crushed ice, adjusting the pH value to 6-7, and filtering to obtain an acetyl ferrocene crude product; and (5) re-crystallizing to obtain the acetyl ferrocene pure product. According to the present invention, the synthesis method has advantages of mild synthesis reaction conditions, easy temperature control, and high yield.

Description

technical field [0001] The application relates to a synthetic method of acetyl ferrocene. Background technique [0002] At present, the synthesis method of α-bromo-acetyl ferrocene is α-bromination reaction of acetyl ferrocene with NBS at low temperature. The α-bromination reaction occurs, and the acylation reaction of bromoacetyl bromide occurs under the catalysis of aluminum trichloride. However, these methods have harsh reaction conditions at low temperature, and have the disadvantages of low yield and difficult post-processing. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of acetyl ferrocene, to overcome the deficiencies in the prior art. [0004] To achieve the above object, the present invention provides the following technical solutions: [0005] The embodiment of the present application discloses a synthetic method of acetyl ferrocene, comprising steps: [0006] (1), acetic anhydride and phospho...

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 Applications(China)
IPC IPC(8): C07F17/02
CPCC07F17/02
Inventor 王明
Owner 苏州天允金属材料有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap