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

A kind of synthetic method of rhodium trifluoroacetate dimer

A technology of rhodium acetate dimer and synthesis method, which is applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation, etc., can solve the problem of entrainment, high cost of raw material rhodium acetate, and incomplete ligand exchange reaction and other problems, to achieve the effect of simple process operation, high product yield and thorough conversion of raw materials

Active Publication Date: 2021-09-21
CHENZHOU GAOXIN PLATINUM +1
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the step of synthesizing rhodium trifluoroacetate with rhodium acetate is relatively simple, the cost of raw material rhodium acetate is high, and the ligand exchange reaction cannot be carried out thoroughly, causing the impurity of raw material rhodium acetate to be brought into the recrystallized product

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

[0027] Dissolve 5.00g of rhodium trichloride hydrate in 100mL of deionized water, stir and heat to 60°C, add dropwise sodium hydroxide solution with a mass fraction of 10% to adjust the pH to 9, age for 20min, and separate rhodium hydroxide precipitate by suction filtration , wash the precipitate with deionized water until there are no chloride ions, stir and disperse the obtained precipitate in 200mL of glacial acetic acid, add 1g of formic acid, react at reflux for 2h at 80°C, evaporate to near dryness under reduced pressure to precipitate blue-green crystals, add to the blue-green solid 90mL of trifluoroacetic acid and 10mL of trifluoroacetic anhydride were heated to reflux for 0.5h, evaporated to nearly dryness under reduced pressure, and dried at 110°C to obtain 5.36g of a green solid with a product yield of 84.93% and a purity of 99.0%.

Embodiment 2

[0029] Dissolve 5.00 g of rhodium trichloride hydrate in 100 mL of deionized water, stir and heat to 60° C., add dropwise a 10% sodium carbonate solution to adjust the pH to 9, age for 20 min, and separate rhodium hydroxide precipitate by suction filtration. Wash the precipitate with deionized water until there is no chloride ion, stir and disperse the obtained precipitate in 200mL of glacial acetic acid, add 1.5g of 37% formaldehyde solution, react at reflux at 70°C for 1.5h, evaporate to near dryness under reduced pressure to precipitate blue-green crystals, and Add 90 mL of trifluoroacetic acid and 10 mL of trifluoroacetic anhydride to the blue-green solid, heat to reflux for 0.5 h, evaporate to near dryness under reduced pressure, and dry at 110°C to obtain 5.39 g of green solid with a product yield of 85.11% and a purity of 99.0%.

Embodiment 3

[0031] Dissolve 5.00 g of rhodium trichloride hydrate in 100 mL of deionized water, stir and heat to 60° C., add dropwise a 10% sodium carbonate solution to adjust the pH to 9, age for 20 min, and separate rhodium hydroxide precipitate by suction filtration. Wash the precipitate with deionized water until there is no chloride ion, stir and disperse the obtained precipitate in 200mL of glacial acetic acid, add 1g of formic acid, reflux at 80°C for 2h, evaporate to near dryness under reduced pressure to precipitate blue-green crystals, add 90mL to the blue-green solid Trifluoroacetic acid and 10 mL of trifluoroacetic anhydride were heated to reflux for 0.5 h, evaporated to nearly dryness under reduced pressure, and dried at 110°C to obtain 5.47 g of a green solid with a product yield of 86.45% and a purity of 99.1%.

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 discloses a method for synthesizing rhodium trifluoroacetic acid dimer: using rhodium trichloride hydrate as a raw material, first synthesizing rhodium hydroxide, then suspending in trifluoroacetic acid containing a reducing agent, heating and refluxing, and reducing the Concentrate under reduced pressure to near dryness, then add trifluoroacetic acid containing trifluoroacetic anhydride, evaporate to near dryness under reduced pressure, and dry the solid in vacuum to obtain rhodium trifluoroacetate dimer. The method of the invention avoids the synthetic route of ligand exchange using rhodium acetate as a raw material, does not bring in rhodium acetate impurities, completes the conversion of raw materials, and has high product yield and good purity; trifluoroacetic acid recovered by vacuum distillation can be used as a reactant Recycling improves the utilization rate of raw materials and reduces environmental pollution; the process is simple and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of organometallic catalyst synthesis, and in particular relates to a synthesis method of rhodium trifluoroacetate dimer. Background technique [0002] Rhodium trifluoroacetate dimer is similar to rhodium perfluorobutyrate dimer (CAS No. 73755-28-9). It is the most electron-deficient compound in rhodium carboxylate dimer, and they are easy to position along the axial direction. Ligand exchange to form rhodium carbene is an important rhodium homogeneous catalyst. There are more and more applications in synthesis, and it has the characteristics of mild reaction conditions, good activity and high selectivity. [0003] For the synthesis of rhodium trifluoroacetate dimer, see "Preparation and Properties of Anhydrous Rhodium(I1) Acetate and Some Adducts Thereof" and "Reactions of Rhodium Trifluoroacetate with Various Lewis Bases. Formation of 4:l Complexes with Pyridine and tert-Butyl In the literature of Isocyanide and Rh...

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): C07C51/41C07C53/18
CPCC07C51/418C07C53/18
Inventor 杨拥军雷婧欧阳文兵叶咏祥雷涤尘杨静
Owner CHENZHOU GAOXIN PLATINUM
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