Pharmaceutical raw material hexafluoroacetone synthesis method

A technology of hexafluoroacetone and synthesis method, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve problems such as complicated process and low final yield, and achieve reduction of intermediate links and shortening of reaction Time, the effect of increasing the reaction yield

Inactive Publication Date: 2018-07-03
CHENGDU DONG DIAN AI ER TECH
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Problems solved by technology

However, most of the existing synthetic methods adopt perfluoroisobutene and potassium permanganate reaction synthesis, the process is more complicated, and the final yield is not very high. There

Method used

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  • Pharmaceutical raw material hexafluoroacetone synthesis method

Examples

Experimental program
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Effect test

example 1

[0010] Add 3mol of 2,3-dihydroxy-hexafluoroisopentane and 4mol of 60% N-methylpropionamide solution into the reaction vessel, increase the temperature of the solution to 70°C, keep it for 60min, and then add 2mol of Bismuth molybdate, continue to react for 50min, lower the temperature to 40°C, and distill under reduced pressure at 10kPa, collect the fraction at 80°C, wash with 70% m-cresol solution, and wash with 80% m-chloroaniline The solution was washed, and the methoxytoluene solution with a mass fraction of 92% was recrystallized to obtain 478.08 g of crystalline hexafluoroacetone, with a yield of 96%.

example 2

[0012] Add 3 mol of 2,3-dihydroxy-hexafluoroisopentane and 5 mol of N-methylpropionamide solution with a mass fraction of 65% in the reaction vessel, raise the temperature of the solution to 75°C, keep it for 70min, and then add 2.5 mol Bismuth molybdate, continue to react for 60min, reduce temperature to 45°C, 15kPa vacuum distillation, collect 85°C cuts, mass fraction is 73% m-cresol solution washing, mass fraction is 82% m-chloroaniline solution washing, The methoxytoluene solution with a mass fraction of 93% was recrystallized to obtain 483.06 g of crystalline hexafluoroacetone, with a yield of 97%.

example 3

[0014] Add 3mol of 2,3-dihydroxy-hexafluoroisopentane and 6mol of 68% N-methylpropionamide solution into the reaction vessel, increase the temperature of the solution to 80°C, keep it for 80min, and then add 3mol of Bismuth molybdate, continue to react for 70min, lower the temperature to 50°C, distill under reduced pressure at 20kPa, collect the cut at 89°C, wash with 76% m-cresol solution, wash with 85% m-chloroaniline solution, mass fraction The methoxytoluene solution with a fraction of 96% was recrystallized to obtain 490.53 g of crystalline hexafluoroacetone with a yield of 98.5%.

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Abstract

The invention relates to a pharmaceutical raw material hexafluoroacetone synthesis method, which mainly comprises: adding 3 mol 2,3-dihydroxy-hexafluoroisopentane and 4-6 mol N-methylpropionamide solution to a reaction container, increasing the temperature of the solution to 70-80 DEG C, maintaining for 60-80 min, adding 2-3 mol bismuth molybdate, continuously carrying out the reaction for 50-70 min, reducing the temperature to 40-50 DEG C, carrying out pressure reducing distillation, collecting the distillate at a temperature of 80-89 DEG C, washing with a metacresol solution, washing with am-chloroaniline solution, and re-crystallizing with a methoxytoluene solution to obtain the crystal hexafluoroacetone.

Description

technical field [0001] The invention relates to a method for synthesizing hexafluoroacetone as a medical raw material. Background technique [0002] Hexafluoroacetone is mainly used as an organic solvent, and it can be copolymerized with ethylene chloride to obtain high-temperature-resistant, corrosion-resistant coatings and adhesives. It is a raw material for the synthesis of medicines, pesticides, polymer materials and organic chemicals. However, most of the existing synthetic methods adopt perfluoroisobutene and potassium permanganate reaction synthesis, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, which is useful for further improving the product quality. Quality and yield, reducing by-product content has important economic significance. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of medical raw material hexafluoro...

Claims

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Application Information

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IPC IPC(8): C07C45/51C07C49/167
CPCC07C45/512C07C49/167
Inventor 严义达
Owner CHENGDU DONG DIAN AI ER TECH
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