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A kind of acetylation method

A technology of ethynylation and acetylenic alcohol, applied in the field of ethynylation, can solve the problems of expensive catalyst, long reaction time, difficult to recycle, etc., and achieve the effect of moderate reaction rate, mild reaction, easy control, and promotion of dissolution

Active Publication Date: 2022-08-05
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] 3. Secondary alkynylation of raw materials forms diol-deficient substances, resulting in waste of raw materials, requiring special treatment and increasing costs
[0015] 4. Catalysts (such as potassium isobutoxide) are expensive and difficult to recycle. The synthesis of alkyne alcohols at low pressure is restricted by the solubility of acetylene, and the reaction time is too long

Method used

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  • A kind of acetylation method
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] First, add N,N-dimethylformamide 126g, sodium methoxide 1.62g (0.03mol), sodium cyanide 0.49g (0.01mol) to the autoclave, seal the autoclave and replace the autoclave with nitrogen three times, and then feed The acetylene was replaced three times, and the acetylene pressure did not exceed 0.15MPa (gauge pressure). Turn on the stirring and set the temperature to 10°C, adjust the pressure of the pressure reducing valve of the acetylene cylinder to 0.1MPa (gauge pressure), and introduce acetylene gas. After the pressure of the reactor is stabilized at 0.1MPa (gauge pressure), use the feed pump to add 6-methyl-5-hepten-2-one 126g (1mol), the feeding time was controlled at 1h. The reaction temperature was controlled to 10°C, and the 6-methyl-5-hepten-2-one feeding was completed and then reacted for 2 hours, and then the pressure was released to release acetylene gas. 60 g of pure water was added to the reaction solution for extraction, the aqueous phase was retained, 30 g o...

Embodiment 2

[0045] First add N,N-dimethylformamide 189g, potassium ethoxide 3.40g (0.05mol), sodium cyanide 1.47g (0.03mol) to the autoclave, use nitrogen to replace the autoclave 3 times after sealing the autoclave, and then feed The acetylene was replaced three times, and the acetylene pressure did not exceed 0.15MPa (gauge pressure). Turn on the stirring and set the temperature to 15°C, adjust the pressure of the pressure reducing valve of the acetylene cylinder to 0.09MPa (gauge pressure), and introduce acetylene gas. After the pressure of the reactor is stabilized at 0.09MPa (gauge pressure), use the feed pump to add 6-methyl-5-hepten-2-one 126g (1mol), the feeding time was controlled at 1h. The reaction temperature was controlled to 15°C, and the 6-methyl-5-hepten-2-one feeding was completed, and the reaction was performed for 2 hours, and the pressure was released to release acetylene gas. 90 g of pure water was added to the reaction solution for extraction, the aqueous phase was ...

Embodiment 3

[0049] First, add N,N-dimethylformamide 189g, sodium ethoxide 0.68g (0.01mol), potassium cyanide 0.325g (0.005mol) to the autoclave, seal the autoclave and replace the autoclave with nitrogen three times, then feed The acetylene was replaced three times, and the acetylene pressure did not exceed 0.15MPa (gauge pressure). Turn on the stirring and set the temperature to 30°C, adjust the pressure of the pressure reducing valve of the acetylene cylinder to 0.08MPa (gauge pressure), and introduce acetylene gas. After the pressure of the reactor is stabilized at 0.08MPa (gauge pressure), use the feed pump to add 6-methyl-5-hepten-2-one 126g (1mol), the feeding time was controlled at 1h. The reaction temperature was controlled to 30°C, the 6-methyl-5-hepten-2-one feeding was completed, and the reaction was performed for 6 hours, and the pressure was released to release acetylene gas. 30 g of pure water was added to the reaction solution for extraction, the aqueous phase was retained...

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Abstract

The present invention provides an acetylation method, using N,N-dimethylformamide as a solvent, inorganic cyanide as a side reaction inhibitor, in the presence of catalyst alkoxide or amino salt, saturated or unsaturated ketone or aldehyde compound The corresponding alkynyl alcohol compounds are obtained through the acetylation reaction, which has the advantages of moderate reaction rate, mild reaction and easy control, easy product separation, and solvent recovery.

Description

technical field [0001] The invention relates to a method for producing VE main intermediate, DV chrysanthemic acid (pyrethroid intermediate), synthesizing vitamin A, vitamin K1, carotenoid intermediate, linalool and other spices and surfactants, in particular to a kind of acetylation The specific method is a method in which a saturated or unsaturated ketone compound is subjected to an ethynylation reaction to obtain a corresponding alkynyl alcohol compound. Background technique [0002] The preparation of corresponding alkynols by acetylenic reaction of saturated or unsaturated ketones is one of the methods for the preparation of intermediates and their chemical products in fine chemical industry. , Vitamin A, vitamin K1, carotenoid intermediates, synthetic rubber monomers, linalool and other spices and surfactants. [0003] Existing acetylene reagents include acetylene Grignard reagent and acetylene gas. Because acetylene Grignard reagent is expensive and generates solid w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/42C07C29/94C07C29/74C07C29/86C07C33/042C07C33/048
CPCC07C29/42C07C29/94C07C29/74C07C29/86C07C33/042C07C33/048
Inventor 鲍元野李康贾峥瑞张永振黎源
Owner WANHUA CHEM GRP CO LTD
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