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Method for preparing methyl cedryl ether from Chinese fir oil

A technology of methyl cedarwood ether and fir oil, which is applied in the direction of ester reaction to prepare ether, ether preparation, metal alcohol preparation, etc. It can solve the problems of rot, waste of resources, and not being well utilized, so as to achieve pure aroma and avoid bumping The effect of punching and coking and shortening the residence time

Active Publication Date: 2014-09-17
江西华晨香料化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Therefore, it is necessary to develop raw materials and apply new technologies, such as using fir as raw material for technological development. As we all know, fir is the most important tree species for afforestation in southern my country, and there are many roots and processing waste left by logging every year. At present, fir roots and processing waste are not well utilized, or left in the mountains to rot, or used for burning, resulting in a waste of resources

Method used

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  • Method for preparing methyl cedryl ether from Chinese fir oil
  • Method for preparing methyl cedryl ether from Chinese fir oil

Examples

Experimental program
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Effect test

Embodiment 1

[0034] In a reaction kettle with a stirring and reflux condenser, add 170ml of toluene and 137g of benzyl sodium, heat to reflux under stirring, add dropwise a solution of 223g of cetaxel and 200ml of toluene, control the temperature of the reaction system to reflux, drop The addition time was 30 minutes, and after the dropwise addition was completed, the reaction was refluxed for 1.5 hours, then cooled to room temperature, and the first step reaction was completed.

[0035] Continue to add 122g of dimethyl sulfate dropwise, and the dropwise addition is completed within 30min. After the dropwise addition, react at 70°C for 2.5h, wash the reaction mixture with 100ml of 10% sodium bicarbonate solution, let stand to separate layers, and separate the water layer , the oil layer was washed with 10% aqueous sodium chloride solution until neutral. Atmospheric distillation first recovers the solvent toluene, and then conducts rectification.

[0036] A superheated steam conduit is arr...

Embodiment 2

[0040]In a reaction kettle with a stirring and reflux condenser, add 195ml of toluene and 182.4g of benzyl sodium, heat to reflux under stirring, add dropwise a solution of 222.4g of cetaxel and 320 ml of toluene, and control the temperature of the reaction system to reflux , the dropwise addition time is 30min, after the dropwise addition is completed, reflux for 1.5h, then cool to room temperature, and the first step reaction is completed.

[0041] Continue to add 151.4g of dimethyl sulfate dropwise, and the dropwise addition is completed within 30min. After the dropwise addition, react at 65°C for 2.5h, wash the reaction mixture with 100ml of 10% sodium bicarbonate solution, let stand to separate layers, and separate the water layer , the oil layer was washed with 10% aqueous sodium chloride solution until neutral. Atmospheric distillation first recovers the solvent toluene, and then conducts rectification.

[0042] A superheated steam conduit is arranged at the bottom of ...

Embodiment 3

[0046] In a reaction kettle with a stirring and reflux condenser, add 100ml of toluene and 114g of benzyl sodium, heat to reflux under stirring, add dropwise a solution of 223g of cetaxel and 250ml of toluene, control the temperature of the reaction system to reflux, drop The addition time was 30 minutes, and after the dropwise addition was completed, the reaction was refluxed for 1 hour, then cooled to room temperature, and the first step reaction was completed.

[0047] Continue to add 151.6g of dimethyl sulfate dropwise, and the dropwise addition is completed within 30min. After the dropwise addition, react at 80°C for 2.5h, wash the reaction mixture with 100ml of 10% sodium bicarbonate solution, let stand to separate layers, and separate the water layer , the oil layer was washed with 10% aqueous sodium chloride solution until neutral. Atmospheric distillation first recovers the solvent toluene, and then vacuum distillation. .

[0048] A superheated steam conduit is arra...

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Abstract

The invention discloses a method for preparing methyl cedryl ether from Chinese fir oil. The method comprises the following steps: by taking Chinese fir oil as a raw material, reacting the separated Chinese fir alcohol with benzyl sodium to obtain Chinese fir alcohol sodium, and reacting for 1-1.5h, wherein the molar ratio of the benzyl sodium to the Chinese fir alcohol is (1.0-1.6):1, the volume ratio of a solvent methylbenzene to the Chinese fir alcohol material in the reaction product is (2-3):1; carrying out methylation on the Chinese fir alcohol sodium and dimethyl sulfate, wherein the molar ratio of the dimethyl sulfate to the dimethyl sulfate is (1-1.2):1; reacting at 60-80 DEG C for 2.4-2.6h, and washing the reaction product by using 10% sodium bicarbonate solution, standing and layering, washing an oil layer to neutral by using 10% sodium chloride solution, and then distilling to obtain the methyl cedryl ether. Compared with a sodium hydride method and a sodium amide method, the method is mild in reaction condition, high in product yield, and pure in fragrance, the methyl cedryl ether prepared from cedar wood oil as a raw material can be replaced with the prepared methyl cedryl ether, and the situation of shortage of cedar wood oil resources can be relieved.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry and relates to a method for preparing synthetic perfume, in particular to a method for preparing methyl cedryl from fir oil. Background technique [0002] Methyl cedryl ether is an important fragrance raw material, which has the smell of ambergris and ointment, and is generally made from cedarwood oil. Yet, adopting cedarwood oil to be raw material to prepare methyl cedryl ether has two deficiencies: [0003] One is that cedarwood oil is distilled from the roots, stems or branches of Cupressaceae plants, and is in great demand in the spice market. Because the growth cycle of cypress is very long, it takes about 60 years to become useful, and cypress resources are scarce, so it is difficult for cypress oil to meet the needs of the spice market. [0004] The second is that the preparation of methyl cedryl ether usually takes the cedryl alcohol obtained by separating cedarwood oil as a ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/18C07C41/16
CPCC07C29/70C07C41/16C07C2603/66C07C43/18C07C35/37
Inventor 俞忠华卜泽平周振华张天古赵建民
Owner 江西华晨香料化工有限公司
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