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Synthesis method of environment-friendly p-methyl anisole

A technology of p-methyl anisole and a synthesis method, which is applied in the directions of ether preparation, ester reaction preparation of ether, organic chemistry, etc., can solve the problems of difficult post-processing, low synthesis yield of methyl anisole, etc., and achieves green synthesis Effect

Active Publication Date: 2017-07-04
山东达冠科技有限责任公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0012] The purpose of the present invention is to solve the problems such as the low synthetic yield of p-methylanisole in the prior art, or the use of toxic and harmful methylation raw materials, or the difficulty in post-processing caused by the use of quaternary ammonium salts that are easily decomposed by heat for phase transfer catalysis. , aiming to provide a green, efficient and economical method for the synthesis of p-methylanisole

Method used

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  • Synthesis method of environment-friendly p-methyl anisole

Examples

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Comparison scheme
Effect test

Embodiment 1

[0033] 54g p-cresol, 100mL DMC, 300mL H 2O, 2g of NaY (1:1 compound) compound and 1g of Turkish red oil were added to the pressure-resistant reactor together, stirred and heated, and when the reaction temperature reached 170°C, the timing was started, and the reaction temperature was controlled to react at 170°C for 3 hours , then cooling, solid-liquid separation, liquid-liquid separation, fractional distillation and concentration of the filtrate to recover the solvent, the content of the concentrated liquid is 99.1% through gas chromatography detection, and the calculated p-methyl anisole yield is 96.3%.

Embodiment 2

[0035] 108g p-cresol, 200mL DMC, 600mL H 2 O, 5g of NaY (1:1 compound) compound and 3g of Turkish red oil were added into the pressure-resistant reactor together, stirred and heated, and when the reaction temperature reached 170°C, the timer was started, and the reaction temperature was controlled to react at 170°C for 3 hours , then cooling, solid-liquid separation, liquid-liquid separation, fractional distillation and concentration of the filtrate to recover the solvent, the concentrated solution is detected by gas chromatography and the yield of p-methyl anisole is calculated to be 97.1%.

Embodiment 3

[0037] Repeat the operation of Example 2, the added water is taken from the separated mother liquor after the reaction in Example 2, no new catalyst is added, and the yield of p-methylanisole is calculated to be 97.3%.

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Abstract

The invention relates to a synthesis method of environment-friendly p-methyl anisole. The method includes: taking p-cresol as the raw material, using a polar solvent like water as the solvent, adopting an alkaline substance Y type zeolite as the catalyst, and adding a proper surfactant Turkey red oil as the emulsifier, and under a 130-180DEG C temperature range and other specific conditions, using environment-friendly dimethyl carbonate (DMC) as the methylation raw material to prepare p-methyl anisole. The yield is up to 96% or above, and the final product purity is up to 99% or more.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a synthesis method of p-methylanisole. Background technique [0002] p-methylanisole (CAS: 104-93-8), also known as 4-methylanisole, p-methoxytoluene, belongs to anisole derivatives. Naturally present in ylang ylang oil and cananga ylang ylang oil, it has the fragrance of violet and ylang ylang flower. It is a very important chemical raw material and is widely used in the fields of medicine, spices and organic synthesis intermediates. This product is an edible spice that is allowed to be used according to GB2760-86 of our country. It is mainly used to prepare walnut, hazelnut and other nut flavors. It is also used in the preparation of artificial essences such as ylang-ylang, cananga, violet, and daffodil. In addition, it can be used as an organic synthesis intermediate to synthesize a series of chemical products such as anisaldehyde. [0003] At present, the synthesis metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/205
CPCC07C41/16C07C43/205
Inventor 张永富徐志华张健雄杨丰科姜云兵
Owner 山东达冠科技有限责任公司
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