A kind of preparation method of acetylenic alcohol

A technology of acetylenic alcohol and acetylene, which is applied in the field of base-catalyzed preparation of acetylenic alcohol, which can solve the problems of affecting product quality and no addition of polymerization inhibitors, and achieve the effects of avoiding polymerization side reactions, shortening reaction time, and improving product yield

Active Publication Date: 2020-01-10
SHANDONG NHU VITAMIN CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that a small amount of co-inhibitor remains in the product, which affects product quality
There is the existence of unsaturated bonds in the acetylenylation reaction, and the polymerization reaction is easy to occur, but there is no report of adding a polymerization inhibitor in the acetylenylation reaction process

Method used

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  • A kind of preparation method of acetylenic alcohol
  • A kind of preparation method of acetylenic alcohol
  • A kind of preparation method of acetylenic alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Under nitrogen protection, add 1.6g PGMA / SiO to a 5L autoclave 2 -TEMPO, then add 798.5g of methyl heptanone and 3.1g of KOH (45wt% solution), and then feed 2.15kg of liquid ammonia into the reaction kettle. The mixture was cooled to 15°C. Then feed 166.8g of acetylene into the autoclave, and control the pressure of the reactor to be 12bar. After reacting for 3.3 hours, carry out solid-liquid separation by filter, then add 25g90% (mass fraction) aqueous acetic acid solution in liquid phase, release pressure, wherein most of ammonia is evaporated, be heated to 40 ℃, remove remaining ammonia. Subsequently, the reaction mixture was washed twice with 250 mL of deionized water, twice with 250 mL of 8% (mass fraction) sulfuric acid aqueous solution, and then twice with 250 mL of deionized water to obtain a colorless transparent liquid.

[0039]The solid phase was applied 7 times, the average conversion rate was 99.3%, the average yield before washing was 98%, the average yi...

Embodiment 2～5

[0047] Experiments were carried out according to the operating conditions in Table 2, and the unlisted conditions were the same as in Example 1, and the yields and selectivities were shown in Table 2.

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Abstract

Disclosed is a method for preparing alkynol, which method comprises subjecting a saturated ketone and acetylene to an ethymylation reaction in liquid ammonia under the action of a polymerization inhibitor and a catalyst, and after the reaction is complete, subjecting same to a post-treatment to obtain the alkynol. The preparation method avoids the occurrence of a polymerization side reaction during the ethymylation reaction, thereby improving the conversion rate of the raw materials and the yield of the alkynol.

Description

technical field [0001] The invention belongs to the technical field of alkali-catalyzed preparation of acetylenic alcohols, and specifically relates to a method in which an alkali metal hydroxide is used as a catalyst and 4-hydroxyl-2,2,6,6-tetramethylpiperidine is supported on silica gel in a reaction kettle. Nitroxide free radicals are a method for preparing acetylenic alcohols through acetylenylation of polymerization inhibitors. Background technique [0002] Alkynyl alcohol is an important intermediate for the synthesis of flavors and fragrances, pharmaceutical intermediates, and vitamin E, such as 3,7-dimethyl-3-octynol, dehydronerolidol, 3,7,11,15-tetramethyl Base-1-hexadecyn-3-ol, etc., due to the prominent position of acetylenic alcohols in the chemical industry, many scholars have conducted a lot of research on their synthetic methods. [0003] CN1125015C adopts cationic exchange resin method to catalyze the synthesis of enynyl alcohol. The method uses weakly acidi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/40C07C29/94C07C33/042
CPCC07C29/40C07C29/94C07C33/042
Inventor 殷宪龙赵德胜黄高峰严宏岳贾文浩赵小川
Owner SHANDONG NHU VITAMIN CO LTD
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