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Purifying process of cyclobutanone

A technology for crude cyclobutanone and cyclobutanone, applied in the separation/purification of carbonyl compounds, organic chemistry, etc., can solve the problems of dichloromethane being volatile, toxic, difficult to separate, etc., and achieve mild conditions for removing impurities. Simple process and cheap effect

Inactive Publication Date: 2013-12-18
HONGSHENG SCI TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that in order to obtain 1kg cyclobutanone, 86kg of dichloromethane needs to be used
Dichloromethane is volatile and toxic, which is harmful to the health of operators and the environment
The boiling point of these impurities is lower or higher than the boiling point of cyclobutanone, which is difficult to separate and seriously affects the use of cyclobutanone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 500g of cyclobutanone crude product (content 90%, GC test) to the 1000ml reaction bottle equipped with agitator and thermometer, add 113g potassium permanganate in four times, control the temperature in the reaction bottle not to exceed 40°C, stir for 4 Hour. After the reaction is complete, add 1000 ml of ether and 500 ml of water, stir, separate the liquids, dry the organic phase, and rectify to collect fractions at 98-99°C with a content of 98.7% (GC test).

Embodiment 2

[0030] Add 500g of crude cyclobutanone (content 95%, GC test) to a 5000ml reaction flask equipped with a stirrer and a thermometer, add 85g of potassium permanganate in two times, control the inner temperature of the reaction flask at 25±2°C, and stir for 3 Hour. After the reaction is complete, add 1000 ml of ether and 500 ml of water, stir, separate the liquids, dry the organic phase, and rectify to collect fractions at 98-99°C with a content of 99.2% (GC test).

Embodiment 3

[0032] Add 500g of crude cyclobutanone (92% content, GC test) into a 1000ml reaction flask equipped with a stirrer and a thermometer, add 106g of chromium trioxide at a time, control the internal temperature of the reaction flask at 30±2°C, and stir for 6 hours. After the reaction is complete, add 1000 ml of ether and 500 ml of water, stir, separate the liquids, dry the organic phase, and rectify to collect fractions at 98-99°C with a content of 99.0% (GC test).

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PUM

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Abstract

The invention relates to a purifying process of cyclobutanone, and aims to provide the purifying process of cyclobutanone simple in method, lower in cost and applicable to industrial production. The purifying process of cyclobutanone comprises the following steps: adding a metal oxidant into a cyclobutanone crude product, and stirring to react for 2-24 hours; rectifying at normal pressure, and collecting fractions at 98-99 DEG C to obtain the product. The purifying process of cyclobutanone provided by the invention has the following advantages that in the whole method, the metal oxidant is just added to stir and react, and the metal oxidant is lowvery cheap in price and is solid at normal temperature and is easy to be separated from organic phases; the whole reaction is not high in temperature (does not exceed 40 DEG C), low in energy consumption and relatively mild in condition of removing impurities; the process can be carried out under a condition of room temperature, so that the process is very applicable to industrial production; the whole process flow is very simple and the purity of cyclobutanone prepared is over 98%.

Description

technical field [0001] The invention relates to a purification process of cyclobutanone. Background technique [0002] Cyclobutanone, English name: Cyclobutanone, molecular formula is C4H6O, is the raw material or intermediate (Adv.Strain Org.Chem., 1991,1,167 and Angew Chem., 1988,10,820) of compound such as preparation penem class medicine. [0003] The preparation method of cyclobutanone usually has two kinds: one is to use cyclobutanol as raw material, oxidize cyclobutanol in water with chromium trioxide and oxalic acid (Organic Synthesis Collective Volumes 7,114-116); Propanethanol is used as raw material. Dissolve cyclopropanol in water, add concentrated hydrochloric acid, and reflux to rearrange cyclopropanol into cyclobutanol, and then oxidize with sodium hypochlorite to obtain cyclobutanone (US6476274). The crude cyclobutanone obtained by the two methods contains and not only contains the following impurities: unreacted cyclopropanol, unreacted cyclobutanol, 3-bute...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/39C07C45/78
Inventor 曾彪
Owner HONGSHENG SCI TECH DEV
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