Preparation method of heptafluoroisobutyl alcohol

A technology of heptafluoroisobutanol and perfluoroisobutyrate, applied in the field of preparation of heptafluoroisobutanol, can solve problems such as hindering the development and development of downstream products, unsuitable for large-scale production, harsh reaction conditions, etc. Promote and solve the effects of high cost and short synthetic route

Pending Publication Date: 2020-11-24
天津长芦新材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods involve the use of dangerous goods, expensive raw materials, harsh reaction conditions, and unsuitability for large-scale production. The further development of , while the research on heptafluoroisobutanol is only in its infancy

Method used

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  • Preparation method of heptafluoroisobutyl alcohol
  • Preparation method of heptafluoroisobutyl alcohol
  • Preparation method of heptafluoroisobutyl alcohol

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Example 1. Methyl perfluoroisobutyrate (30g) was dissolved in anhydrous methanol (30mL), cooled to 0°C, sodium methoxide (7.3g) was added, and after stirring in an ice-water bath for 30 minutes, boron was slowly added in batches Sodium hydride (5 g) was added and stirred evenly, and the reaction was carried out at room temperature for 10 h, and the reaction was completed as detected by infrared spectroscopy. The solvent of the reaction solution was first distilled off, then washed with brine, dried over sodium sulfate, and concentrated to obtain the product heptafluoroisobutanol (20 g) with a yield of 76%.

Embodiment 2

[0018] Example 2. Methyl perfluoroisobutyrate (300g) was dissolved in anhydrous methanol (300mL), cooled to 0°C, sodium methoxide (73g) was added, and after stirring in an ice-water bath for 30 minutes, hydroboration was slowly added in batches Sodium (50g), stir evenly after the addition, react at room temperature for 10h, and the reaction is complete as detected by infrared spectrum. The solvent of the reaction solution was first distilled off, then washed with brine, dried over sodium sulfate, and concentrated to obtain the product heptafluoroisobutanol (220 g) with a yield of 83%.

Embodiment 3

[0019] Example 3. Dissolve ethyl perfluoroisobutyrate (60g) in anhydrous methanol (60mL), cool to 0°C, add sodium methoxide (13g), stir in an ice-water bath for 30 minutes, slowly add hydroboration in batches Sodium (4.5g), stir evenly after the addition, react at room temperature for 10h, and the reaction is complete as detected by infrared spectrum. The solvent of the reaction solution was first distilled off, then washed with brine, dried over sodium sulfate, and concentrated to obtain the product heptafluoroisobutanol (37 g) with a yield of 75%.

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Abstract

The invention belongs to the field of fluorine chemical industry, and particularly relates to a preparation method of heptafluoroisobutyl alcohol. The preparation method comprises the following steps:adding raw material perfluoroisobutyrate, solvent methanol and organic base assistant into a reaction vessel; performing cooling in an ice-water bath, then adding solid sodium borohydride by using aspiral feeder to react, and after the feeding is completed, recovering the room temperature to carry out stirring reaction; and after the reaction is finished, performing distilling to remove the solvent in the reaction solution, performing washing with saline solution, drying with sodium sulfate, and performing concentrating to obtain the product. Through the conventional chemical reduction reaction, no dangerous reagent is used, the synthetic route is short, the post-treatment is simple, and the reaction yield is high, so that the product can be produced on a large scale, and is low in priceand convenient to popularize.

Description

technical field [0001] The invention belongs to the field of fluorine chemical industry, in particular to a preparation method of heptafluoroisobutanol. Background technique [0002] Heptafluoroisobutanol is a new type of fluorocarbon material, which can be used as an important intermediate for the synthesis of new medicines, pesticides, fabric finishing agents and fragrances. It can also be used as an important organic solvent and as a new organic polymer. The raw materials or additives of materials have great market prospects and development value. [0003] At present, there are several preparation methods for its isomer heptafluorobutanol: (1) Lithium aluminum hydride reduces perfluoroalkyl carboxylic acid to perfluoroalkyl alcohol; (2) Perfluoro aliphatic aldehyde reacts with Grignard reagent to form Alcohol;, (3) hexafluoropropene reacts with hydrogen fluoride in formaldehyde solution. However, these methods involve the use of dangerous goods, expensive raw materials,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/147C07C31/38
CPCC07C29/147C07C31/38
Inventor 刘亚欣张志君陈爽徐雅硕马雅松
Owner 天津长芦新材料研究院有限公司
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