Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology of pentafluorophenol and toluene, applied in the field of preparation of pentafluorophenol, can solve the problems of high manufacturing cost, waste of bromine resources, environmental pollution and the like
Active Publication Date: 2020-07-07
上海万溯药业有限公司 +1
View PDF3 Cites 0 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
This method uses bromopentafluorobenzene as the raw material for introducing pentafluorophenyl, which also has defects such as waste of bromine resources, low atom economy, environmental pollution, and high manufacturing costs.
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
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
preparation example Construction
[0053] The first aspect of the present invention provides a kind of preparation method of pentafluorophenol, the structure of described pentafluorophenol is as shown in formula I:
[0054]
[0055] The preparation method of pentafluorophenol provided by the present invention can comprise decarboxylation reaction, and described decarboxylation reaction is specifically: the compound of formula II is under the condition that alkali exists, generates the compound of formula III, and reaction equation is as follows:
[0056]
[0057] In the decarboxylation reaction, the reaction can usually be carried out under the condition of gas protection, and the gas protection can use one or more combinations of nitrogen, inert gas, etc., and the inert gas can be, for example, helium, neon , argon, krypton, xenon, etc. one or more combinations.
[0058] In the decarboxylation reaction, the reaction can be carried out in the presence of a reaction solvent, which can be an organic solvent...
Embodiment 1
[0083] 1L three-necked flask, add 424 grams of pentafluorobenzoic acid, 1060 grams of toluene, and 202 grams of triethylamine. Heating to 100°C-110°C, reacting for 24 hours, the conversion is complete. Atmospheric pressure recovery triethylamine and toluene. Distilled to obtain 335g of pentafluorobenzene, GC area normalization method purity (A%): 99%, yield: 99%. GCMS: 168.
Embodiment 2-6
[0085] The consumption and kind of organic solvent are as shown in table 1, and other is with embodiment 1, and its result is shown in table 1
[0086] Table 1
[0087]
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
Login to view more
Abstract
The invention relates to the field of organic synthesis and in particular relates to a preparation method of pentafluorophenol. The structural formula of pentafluorophenol is as shown in a formula I. The preparation method specifically comprises the following steps of: (1) decarboxylic reaction; (2) Grignard reaction; and (3) oxidizing reaction. According to the preparation method of pentafluorophenol, raw materials are easily available and are low in cost, the production cost is low, the waste of bromine resources is avoided, and adverse effects on the environment are reduced; meanwhile, the preparation method of pentafluorophenol is mild in reaction condition, high in process safety, few in product impurity, easy in extraction and purification and stable in quality; and the content of pentafluorophenol obtained by refining is greater than 99%, so that the preparation method is completely suitable for large-scale industrial production.
Description
technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of pentafluorophenol. Background technique [0002] Pentafluorophenol is an important chemical intermediate widely used in the fields of medicine and liquid crystal materials, so it has become the research and development focus of various pharmaceutical companies and chemical companies. [0003] At present, there are the following several reports on the preparation method of pentafluorophenol in the world: [0004] 1. Foreign literature uses hexafluorobenzene as a raw material and hydrolyzes pentafluorophenol under alkaline conditions to produce pentafluorophenol (Journal of Organic Chemistry; vol.56; nb.26; (1991); p.7350–7354). The manufacturing cost of this method is too high to meet the market price demand. [0005] 2. CN102887817 uses pentafluorobromobenzene as the raw material for introducing pentafluorophenyl, that is, pentafluorobromobenzene is acid...
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
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to view more 
Login to view more