Method employing a-pinene to prepare 2,3-epoxy pinane

A technology of pinene oxide and pinene is applied in the chemical field, and can solve the problems of easy explosion, low yield of pinene oxide, unstable peracetic acid, etc., and achieves reduction of production cost, improvement of yield, and elimination of explosion. the dangerous effect of

Inactive Publication Date: 2014-06-04
SOUTHWEST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, peroxybenzoic acid is used as oxidant, and the yield of 2,3-epoxy pinane is 80%, but the cost of peroxybenzoic acid is higher; if 40% peroxyacetic acid is used as oxidant, 2,3-epoxy pinane The yield of pinane can be increased to 85%, however, 40% peracetic acid is unstable and prone to explosion in the preparation process, making it inconvenient to produce
Therefore, someone tried to use 20% peracetic acid as an oxidizing agent, and the yield of pinane epoxy was as low as 60-65%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 0.1mol of α-pinene, 25mL of chloroform, and 12.72g of anhydrous sodium carbonate into a four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, and a condenser to prepare solution I, and then add Tetrabutylammonium bromide and load-type mesoporous molecular sieve catalyst, make the concentration that tetrabutylammonium bromide accounts for in solution I be 0.02mol / L, the consumption of load-type mesoporous molecular sieve catalyst is α-pinene quality 3%, the catalyst is a mesoporous molecular sieve loaded with 40% phosphotungstic acid, add dropwise peracetic acid with a concentration of 18% under stirring, the dosage of peracetic acid is 0.2mol, cool with cold water, and the temperature is controlled at 4°C. 3h;

[0026] Pour the product into a funnel first, and perform suction filtration first to obtain the filtrate and filter cake; add 200 mL of water to wash the filter cake, collect the washing liquid, leave the washing liquid to separate lay...

Embodiment 2

[0028] Add 0.1 mol of α-pinene, 25mL of chloroform, and 12.72g of anhydrous sodium carbonate into a four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, and a condenser to prepare solution I, and then add Tetrabutylammonium bromide and load-type mesoporous molecular sieve catalyst, make the concentration that tetrabutylammonium bromide accounts for in solution I be 0.08mol / L, the consumption of load-type mesoporous molecular sieve catalyst is α-pinene quality 3.5% (0.476g), the catalyst is a mesoporous molecular sieve loaded with 40% phosphotungstic acid, add dropwise peracetic acid with a concentration of 18% under stirring, the dosage of peracetic acid is 0.35mol, cool with cold water, and the temperature is controlled at 16°C, react for 2.5h;

[0029] Pour the product into a funnel first, and perform suction filtration first to obtain the filtrate and filter cake; add 200 mL of water to wash the filter cake, collect the washing liquid, leave the wash...

Embodiment 3

[0031] Add 0.1mol of α-pinene, 25mL of chloroform, and 12.72g of anhydrous sodium carbonate into a four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, and a condenser to prepare solution I, and then add Tetrabutylammonium bromide and load-type mesoporous molecular sieve catalyst, make the concentration that tetrabutylammonium bromide accounts for in solution I be 0.06mol / L, the consumption of load-type mesoporous molecular sieve catalyst is α-pinene quality 2% (0.272g), the catalyst is a mesoporous molecular sieve loaded with 40% phosphotungstic acid, add dropwise peracetic acid with a concentration of 18% under stirring, the dosage of peracetic acid is 0.35mol, cool with cold water, and the temperature is controlled at 16°C, react for 2.5h;

[0032] Pour the product into a funnel first, and perform suction filtration first to obtain the filtrate and filter cake; add 200 mL of water to wash the filter cake, collect the washing liquid, leave the washing...

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PUM

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Abstract

The invention provides a method employing a-pinene to prepare 2,3-epoxy pinane; the method comprises the following steps: 1, preparing reaction solution; 2, droping peroxyacetic acid with concentration at 18% under stirring condition to the reaction solution for reaction, and the temperature of the reaction liquid is controlled to be under 20 DEG C; 3, carrying out pumping filtration to reaction products of the step 2 so as to obtain filter liquid and filter cake; 4, adding 200mL water to clean the filter cake, collecting filter liquid standing and layering the filter liquid, and isolating a water layer from an organic layer; 5, using saturation sodium chloride solution and saturation sodium hyposulfite solution to clean the organic layer for once in order, using the saturation sodium chloride solution to clean the organic layer to a middle layer, using waterless sodium sulfate to dry, and evaporating solvent in normal temperature to obtain the product. The method improves yield of the 2,3-epoxy pinane, reduces production cost, and simultaneously removes the danger of employing high density peroxyacetic acid to cause explosion.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing 2,3-epoxy pinane by using α-pinene. Background technique [0002] The epoxidation of α-pinene under the action of organic peroxyacids to synthesize fragrance intermediates is an important route in organic synthesis and fragrance chemistry. At present, peroxybenzoic acid is used as oxidant, and the yield of 2,3-epoxy pinane is 80%, but the cost of peroxybenzoic acid is higher; if 40% peroxyacetic acid is used as oxidant, 2,3-epoxy pinane The yield of pinane can be increased to 85%. However, 40% peracetic acid is unstable and prone to explosion during the preparation process, which is inconvenient for production. Therefore, someone tried to use 20% peracetic acid as an oxidant, and the yield of pinane epoxy was as low as 60-65%. Contents of the invention [0003] The purpose of the present invention is to solve the defects in the above-mentioned prior art...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/04C07D301/14
CPCC07D301/14C07D303/04
Inventor 吴春华朱丹丹秦永剑代学宇刘慧青张加研杜官本
Owner SOUTHWEST FORESTRY UNIVERSITY
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