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Preparation method of methyl eugenol

A technology of eugenol methyl ether and eugenol, which is applied in the field of preparation of eugenol methyl ether, can solve the problems of low product purity, inability to balance yield and cost, etc., and achieve benefits to yield, reduce energy consumption, and save costs Effect

Active Publication Date: 2013-11-27
CHONGQING THRIVE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is: the yield and the cost of the preparation method of the existing eugenol methyl ether cannot be balanced, the product purity is low, and a large amount of organic solvents are used in the production process

Method used

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  • Preparation method of methyl eugenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The preparation method of a clove phenolin, including the following steps:

[0042] a. Match 8.4g of sodium hydroxide and 75g of water into about 10%concentration of alkali and add it to the reactor, stir down and add 24.6g clove phenol;

[0043] b. The reaction temperature is controlled at 20 ° C, and slowly dripped 22.8g of sulfate dihydrin under fierce stirring, about 1h drop;

[0044] c. After dripping, after the stirring reaction is 1h, the increase temperature to 40 ° C reacts 1h to decompose sulfuric acid dihydrin;

[0045] d. Subticiency, organic phase decompression distillation is the product.

[0046] The product is 24.87g of colorless transparent liquid, and the yield is 93.0%, such as figure 1 The GC purity is 99.53%.

Embodiment 2

[0048] The preparation method of a clove phenolin, including the following steps:

[0049] a. Match 9.6g of sodium hydroxide and 90g of water into about 10%concentration of alkali solution and add the reactor, stir down and add 24.6g clove phenol;

[0050] b. The reaction temperature is controlled at 20 ° C, and slowly dripped 22.8g of sulfate dihydrin under fierce stirring, about 1h drop;

[0051] c. After dripping, after the stirring reaction is 1h, the increase temperature to 40 ° C reacts 1h to decompose sulfuric acid dihydrin;

[0052] d. Subticiency, organic phase decompression distillation is the product.

[0053] The product is 25.37g of colorless transparent liquid, and the yield is 94.9%, such as figure 2 The GC purity is 99.53%.

Embodiment 3

[0055] The preparation method of a clove phenolin, including the following steps:

[0056] a. Match 16.8g of sodium hydroxide and 150g of water into about 10%concentration of alkaline solution and add the reactor, stir down and add 49.2g clove phenol;

[0057] b. The reaction temperature is controlled at 20 ° C, and slowly dripped and add 45.6g of sulfate diacerne, about 1.5h dripping;

[0058] c. After dripping, after the stirring reaction is 1h, the increase temperature to 50 ° C reacts 1h to decompose sulfuric acid dihydrin;

[0059] d. Subticiency, organic phase decompression distillation is the product.

[0060] The product is colorless transparent liquid 49.1g, and the yield is 91.8%, such as image 3The GC purity is 99.45%.

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Abstract

The invention belongs to the field of organic synthesis and particularly relates to a preparation method of methyl eugenol. The preparation method of the methyl eugenol comprises the following steps: a, adding right amount of sodium hydroxide solution into a reaction kettle, and dripping right amount of eugenol under a stirring condition; b, keeping stirring, controlling the reaction temperature to be 20 to 30 DEG C, slowly dripping excess methyl sulfate; c, after dripping, stirring for 1 h reaction continuously, and increasing the temperature to be 40 DEG C to 50 DEG C for 1 h reaction for resolving the methyl sulfate; d, dividing liquid, carrying out underpressure distillation to organic phases so as to obtain a product. The preparation method provided by the invention solves the problems of incapability of considering the yield and the cost at the same time and low product purity in a conventional preparation method of the methyl eugenol, and has the advantages of high yield, high product purity and low cost.

Description

Technical field [0001] The present invention is an organic synthetic field, especially the preparation method of clove phenol methar ether. Background technique [0002] Cycralol methyl ether, also known as methyl butcxol, English name (Eugenol Methyl Ether), chemical name is 1,2-di oxygen-4- (2-acryl) benzene, molecular formula is C11H14O2, and the structure is: [0003] [0004] The molecular weight is: 178.23, boiling point: 244-245 ° C, relative density: 1.032-1.036, refractive index: 1.532-1.536, flash point: 99 ° C.Colorless to slightly yellow liquid, almost insoluble in water, soluble in 70 % ethanol with 1: 2.Naturally, it exists among high -grained plants such as BlackBerry, Pepper, Circle Angelica, Fine Leaf Enchida, and Lemon Bald. [0005] Cycralphenolin has a sweet lilac-fennel aroma, like a fragrant stone, and the aroma is more transparent and long-lasting. There is a gentle sprout of tea-like, which can be used as a liplabitone's aroma lift;The oriental fragrant ...

Claims

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Application Information

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IPC IPC(8): C07C43/215C07C41/16
Inventor 季卫刚赵华文刘端唐凌洪伟
Owner CHONGQING THRIVE CHEM
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