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Method for preparing epoxy pinane using sodium percarbonate as reagent

A technology of sodium percarbonate and epoxy pinane, which is applied in the direction of organic chemistry, can solve the problems of low purity and low yield of epoxy pinane, and achieve the effect of improving purity, low price, and avoiding ring-opening rearrangement

Inactive Publication Date: 2003-06-11
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Above-mentioned method has its strengths and weaknesses respectively, most of them method, the productive rate of product epoxy pinane is on the low side and the purity is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 136g (1 mole) α-pinene, 250g (available oxygen content of 12%) sodium percarbonate and 1000mL dichloromethane were added to a 2000mL three-necked flask. 200 mL of acetic anhydride was added with vigorous stirring, and the reaction was kept under reflux conditions. After the addition, continue stirring at room temperature, and use GC to track the reaction until the α-pinene reaction is completed, which usually takes 20 to 24 hours. The inorganic solids are removed by filtration, and the reaction mixture is used to remove residual peroxy compounds by conventional methods. After recovering the solvent, rectify and collect the fraction at 102-5°C / 7Kpa. The α-epoxy pinane has a yield of 85-90%, a purity of >95%, and a cool fragrance.

Embodiment 2

[0022] A 500mL three-necked flask was charged with 34g β-pinene, 50g sodium percarbonate, 150mL benzene and 3g triethylbenzylammonium chloride (TEBA). Under vigorous stirring, 45 mL of acetic anhydride was added, and the reaction temperature was controlled below 40°C. After the addition, continue to stir the reaction at room temperature and use GC to track until the β-pinene reaction is completed, which usually takes 18-20 hours. The reaction mixture was processed according to the method of Example 1 to obtain β-epoxypine, with a yield of 80-90% and a purity of >95%.

Embodiment 3

[0024] A 500mL three-necked flask was charged with 34g α-pinene, 50g sodium percarbonate, 150mL toluene and 2.5g PEG-200 (the amount of PEG-400 was 5g, and the amount of PEG-600 was 7.5g). Under vigorous stirring, 40 mL of acetic anhydride was added, and the reaction temperature was controlled below 60°C. After the addition, continue to stir at room temperature, and use GC to track the reaction until the α-pinene reaction is completed, which usually takes 15 to 20 hours. The reaction mixture was processed according to the method of Example 1, and the yield of α-epoxypinene was 85-90%, and the purity was >95%.

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PUM

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Abstract

The invention is a method to prepare epoxy pinane from pinane using sodium percarbonate as agent. It uses the sodium percarbonate as agent, adds acetic anhydride at reaction time, adds phase-transferring catalyzer in need, controls the reaction below 60 C degree for 1-24 hours and obtains epoxy pinane.

Description

Technical field [0001] The present invention is a method for preparing epoxy pinane by using sodium percarbonate as a reagent. Background technique [0002] Pinene is an important component of turpentine, and our country has abundant natural resources. Because of the difference in the position of the double bond in the molecule, there are α-pinene and β-pinene. Due to its very active chemical properties, pinene is an important raw material in the perfume industry and can produce a series of widely used perfumes. Among them, the epoxy pinane produced by the epoxidation reaction of α-pinene is a useful intermediate in the perfume and pharmaceutical industries. Such as α-epoxy pinane in ZnCl 2 Under the action of ring opening and rearrangement, camphor aldehyde is obtained, which can be condensed with a variety of carbonyl compounds to produce a series of sandalwood products (US4052341, CH629461, 629462, etc.), which are widely used in the perfume industry. The ring-opening product ...

Claims

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Application Information

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IPC IPC(8): C07D301/14C07D303/06
Inventor 丁宗彪陆文聪王全瑞陶凤岗胡建良杨育青
Owner FUDAN UNIV
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