An alkynol preparing method

A technology of acetylenic alcohol and acetylene, which is applied in the field of chemical intermediate preparation, can solve the problems of difficult stability of single substitutions and low yield, and achieve the effects of increasing yield, increasing safety, and eliminating the existence of air

Active Publication Date: 2015-07-01
SHANGYU NHU BIOCHEM IND +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are also Japanese documents pointing out the method of using magnesium and Grignard transfer method to prepare monoacetylene magnesium compound for addition, but there are insurmountable shortcomings such as low yield and difficult stable existence of single substitutions.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] (1) In a 500ml glass reactor to be pressed with a FTIR (Fourier transform infrared spectrometer) probe and a thermometer, add 4.8g of magnesium flakes, and then add 300ml of diethyl ether containing 21.8g of bromoethane. Stir until the magnesium flakes disappear (you can add a small amount of iodine to initiate). Then lower the temperature to -10°C and slowly pass through acetylene without acetone until it turns white. Close the vent and raise the acetylene pressure to 3.0 bar. React until there is no acetylene gas absorption, and the FTIR curve scan shows that the peak height of the bilateral acetylene disappears, and the unilateral acetylene product is obtained;

[0058] (2) Keep the acetylene pressure at 3.0 bar and the kettle temperature at about 0°C, slowly pump 13 g of methyl vinyl ketone (content 99.5%) into the reaction system of step (1). After that, react for 1 h. Return to normal pressure, keep the reaction solution at about 0°C and slowly drop in 10% dilu...

Embodiment 2

[0060] The operation method is basically the same as in Example 1, except that the methyl vinyl ketone in step (2) in Example 1 is replaced by β-ionone, the reaction temperature is 5°C, and the hydrolysis temperature is 5°C. Ethynyl-β-ionol was obtained with a yield of 96% after post-treatment.

Embodiment 3～7

[0062] The reaction conditions of Examples 3-7 are basically the same as those of Example 1, the substrate and pressure are as shown in Table 1, and the results obtained are listed in Table 1.

[0063] The reaction conditions and the result of embodiment 3~7

[0064] Example

[0065] 7

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PUM

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Abstract

An alkynol preparing method is disclosed. The method includes: (1) feeding acetylene into a metal agent to perform a metal exchanging reaction, after the reaction is finished, controlling the pressure of the acetylene to be 0.3-1.5 MPa, performing a unilateral reaction, and obtaining a unilateral acetylide through online infrared monitoring; and (2) maintaining the pressure of the acetylene to be 0.3-1.5 MPa, adding a carbonyl compound into the unilateral acetylide obtained in the step (1), performing an addition reaction, and after the addition reaction is finished, hydrolyzing to obtain the alkynol. In the preparing method, the pressure of the acetylene is maintained in a proper range, so that the ratio of the unilateral acetylide in the unilateral reaction is controlled, and the yield of the finally obtained alkynol is further increased.

Description

technical field [0001] The invention belongs to the field of preparation of chemical intermediates, and in particular relates to a preparation method of acetylenic alcohol. Background technique [0002] The ethynylation process of carbonyl groups has been studied very early. In 1947, the US2425201 patent described the use of metal calcium to form acetylene calcium in liquid ammonia and acetylene, and the obtained acetylene calcium reacted with carbonyl compounds to obtain alkynes after hydrolysis. Alcohol compounds. It was later found that many alkali metals can form acetylides in liquid ammonia, and can form acetylenic alcohols with carbonyl compounds. However, for unsaturated carbonyl compounds, such as methyl vinyl ketone, it is easy to polymerize in the alkaline environment of liquid ammonia, resulting in a sharp drop in yield. [0003] The Roche company in 1976 also invented the reaction of using magnesium and sodium amides to replace in US3985817. The magnesium and ...

Claims

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Application Information

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IPC IPC(8): C07C29/42C07C33/042C07C33/048C07C33/14
Inventor 王志轩吴兴华李寅李波
Owner SHANGYU NHU BIOCHEM IND
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