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A kind of synthetic method of 1-octen-3-ol

A synthesis method and technology for octene, applied in the field of chemistry, can solve problems such as easy explosion, complexity, production limitation of 1-octene-3-ol, etc., and achieve the effects of improving safety and reducing fire accidents

Active Publication Date: 2016-03-23
WUTONG AROMA CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main synthetic methods of this compound are: 1) prepare 1-octen-3-alcohol by the reaction of Grignard reagent, but this method needs to use a large amount of ether, unsafe and complicated reaction condition; 2) by aldol condensation method Preparation of 1-octen-3-ol, but this method uses sulfur-containing compounds that are difficult to remove, and is not suitable for food and cosmetics
As early as 1983, scientists such as S.WNUK proposed to prepare 1-octen-3-ol through the reaction of Grignard reagent and aldol condensation, but the production of 1-octen-3-ol was limited due to the above problems
And when ether is in use, it is easy to produce peroxide due to exposure to light or contact with air. When peroxide exists, the distillation temperature of the solvent is higher than 100°C, which is prone to explosion hazards.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The synthetic method of 1-octen-3-ol comprises the following steps:

[0033] 1) Install a 1000mL reaction flask equipped with a stirring device, with a dropping funnel on the top (the reaction system should be fully and strictly dried before the reaction), and a heating mantle at the bottom as a heating source. First, 280 g of anhydrous methyl tert-butyl ether and 16.5 g of magnesium particles (the purity of the magnesium particles are 99.5%) were put into the reaction flask. Turn on the temperature of stirring and heating system to reflux, about 55 ℃, when there is reflux phenomenon, stop stirring, add the mixed solution (94g bromopentane+ 55g of anhydrous methyl tertiary butyl ether is mixed, mol ratio 1:1), bromopentane: magnesium particles=1:1.1, mol ratio, then start stirring, when the end of the cooler has an obvious reflux phenomenon, explain The reaction has already started. At this time, wait quietly until the reflux at the end of the condenser is stable, indi...

Embodiment 2

[0037] The synthetic method of 1-octen-3-ol comprises the following steps:

[0038] 1) Install a 1000mL reaction flask equipped with a stirring device, with a dropping funnel on the top (the reaction system should be fully and strictly dried before the reaction), and a heating mantle at the bottom as a heating source. 280 g of anhydrous methyl tert-butyl ether and 16.5 g of magnesium particles (the purity of the magnesium particles is 98.5%) were put into the reaction flask. Open the temperature of stirring and heating system to reflux, about 55 ℃, when there is reflux phenomenon, stop stirring, in reaction flask, add the mixed solution (102g bromopentane+ The anhydrous methyl tertiary butyl ether of 60g is mixed, mol ratio is 1:1), bromopentane: magnesium particle=1:1, then start stirring, when the end of the cooler has obvious reflux phenomenon, it shows that the reaction has started At this time, you should wait quietly until the reflux at the end of the condenser is stabl...

Embodiment 3

[0042] The synthetic method of 1-octen-3-ol comprises the following steps:

[0043]1) Install a 1000ml reaction flask equipped with a stirring device, with a dropping funnel on the upper part (the reaction system should be fully and strictly dried before the reaction), and a heating mantle as a heating source at the bottom. 280 g of anhydrous methyl tert-butyl ether and 16.5 g of magnesium particles (purity of magnesium particles: 99.2%) were put into the reaction flask. Open the temperature of stirring and heating system to reflux, about 55 ℃, when there is reflux phenomenon, stop stirring, add the mixed solution (98g bromopentane+ 57g of anhydrous methyl tertiary butyl ether is mixed, mol ratio 1:1), bromopentane: magnesium particles=1:1.05, then turn on stirring, when the end of the cooler has obvious reflux phenomenon, it shows that the reaction has started At this time, you should wait quietly until the reflux at the end of the condenser is stable, indicating that the re...

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Abstract

The invention discloses a synthesis method of 1-octylene-3-alcohol. The method comprises the following steps: (1) generating a Grignard reagent by virtue of reaction of bromopentane and maganesium; (2) generating 1-octylene-3-alcohol by virtue of reaction of the Grignard reagent and acrolein; and (3) carrying out after-treatment, namely stirring and hydrolyzing the 1-octylene-3-alcohol at the temperature of -2 to 3 DEG C, adjusting the pH value to be 1-5, carrying out vapor distillation, collecting distilled products at a boiling range of 60 to 65 DEG C under the pressure of 800Pa, and collecting the distilled products in different phases, thereby obtaining the 1-octylene-3-alcohol. The method is simple in process and high in yield, and waste water can be partially recycled.

Description

technical field [0001] The invention belongs to the field of chemistry, and particularly relates to a method for synthesizing 1-octen-3-ol. Background technique [0002] The CAS registration number of 1-octen-3-ol is: 3391-86-4; Chinese alias: mushroom alcohol. English name: 1-Octen-3-ol; alias Flowtronmosquitoattractant; Morillol; Mushroomalcohol; Octen-3-ol; Pentylvintylcarbinol. Density 0.84g / ml, boiling point 84-85°C (25mmHg), refractive index n20 / D=1.437. Molecular formula: C8H16O, molecular weight: 128.212, structural formula such as figure 1 shown. [0003] 1-Octen-3-ol is commonly known as pine alcohol and mushroom alcohol. It is named after it was found in Japanese pine. It is an oily liquid with mushroom fragrance and strong loam and herbal aroma. It exists in natural In plants, it also exists in the flavor substances of peppermint essential oil, lavender essential oil, and cereals. Its safe use is FDA121.1164 and FEMA2805, so it is used in beverages, candies,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/03C07C29/40
CPCC07C29/40C07C33/03
Inventor 李新李磊磊自妍妍卫洁王立志毛浙徽臧传近郭鸽陈祥张雷亮
Owner WUTONG AROMA CHEM CO LTD
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