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Method for aromatizing synthetic oak moss

A technology for synthesizing oak moss and aromatizing, which is applied in the field of aromatizing synthetic oak moss, can solve the problems that the color of salt water is not easy to handle and is not suitable for recycling, etc., and achieves the effect of simple post-processing procedure and easy recovery.

Active Publication Date: 2018-12-28
兰州馥尔盛科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The patent CN106631794A of International Spices and Essences Company is a preparation process of oakmoss crystal spices. It adopts a one-pot method to synthesize oakmoss crystals. This method uses methanol as a solvent and needs to add water. Aromatization produces methyl chloride, which is not suitable for recovery because the boiling point of methyl chloride is only -22°C

Method used

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  • Method for aromatizing synthetic oak moss

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 200g of 2,5-dimethyl-dihydro-resorcinate methyl ester, 400g of water, and 400g of dichloromethane into a 2000ml four-necked bottle, and feed 800g of chlorine gas at 0-25°C, then separate the organic phase, Clean the dichloromethane in the organic phase, add 300g of acetonitrile, and after aging at 80°C for 5 hours, recover 200g of acetonitrile, cool down and filter with suction to obtain the crude oakmoss, and obtain a filter cake after drying to obtain 113g of the product, with a purity of 98.2% yield 90.9%.

Embodiment 2

[0026] 200g 2,5 dimethyl-dihydro-resorate methyl ester (containing the neutralized sodium chloride in the Michael addition reaction) and 400g methylene chloride and the water separated in the example 1 are added in the 2000ml four-necked bottle , at 0-25°C, feed 800g of chlorine gas, then separate the organic phase, collect the dichloromethane in the organic phase, add 600g of acetonitrile, react at 85°C for 10 hours, then recover 450g of acetonitrile, cool down and filter to obtain the synthetic The crude oak moss was dried to obtain 112.5 g of the product, with a purity of 98.1% and a yield of 90.5%.

Embodiment 3

[0028] 200g 2,5 dimethyl-dihydro-resorate methyl ester (containing the neutralized sodium chloride in the Michael addition reaction) and 600g methylene chloride and the water separated in the example 2 are added in the 2000ml four-necked bottle , at 0-25°C, feed 800g of chlorine gas, then separate the organic phase, filter the water phase, filter the sodium chloride to collect dichloromethane in the organic phase, add 900g of acetonitrile, react at 86°C for 18 hours, and then recover the acetonitrile 790g, cooled to 10°C, and then suction-filtered to obtain the crude oak moss product, which was dried to obtain 110g of the product, with a purity of 98.6% and a yield of 88.5%.

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Abstract

The invention provides a method for aromatizing synthetic an oak moss. The method comprises the following steps: adding chlorinated 2,5dimethyl-dihydro-methyl resorcylate into a solvent acetonitrile for aromatization reaction; then carrying out cooling crystallization to obtain a coarse product of the synthetic oak moss. Compared with the prior art, the method for aromatizing the oak moss, disclosed by the invention, has the following advantages: firstly, the by-product sodium chloride produced by the reaction can be directly filtered; secondly, reactive water can be recycled; thirdly, when the aromatization reaction is carried out, the reaction is not drastic because the reaction occurs in the acetonitrile solvent, and the generated hydrogen chloride is easy to recover; fourthly, an aftertreatment process is simple and the purity of the produced crude product reaches 98 percent or above. Therefore, the method provides an improved process method for the synthetic oak moss, which is environmentally friendly and energy saving and can be used for industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to an improved method for aromatizing synthetic spices, in particular to a method for synthesizing oakmoss aromatizing. Background technique [0002] Oakmoss has a unique oakmoss-like fragrance monomer and a good fixative, and is widely used in soaps, detergents, high-end perfumes and tobacco. In the past, natural oak moss extract was used, which changed color when it met alkali, and it was difficult to prepare soap essence. If synthetic oak moss is used, there will be no such disadvantages. [0003] The synthetic method of oakmoss at present, has reported in West Germany published patent 2,359,233 (1974) and is made raw material with dimethyl malonate, condenses in the methanol solution of sodium methylate and obtains the dihydro oakmoss intermediate, and then Using reagents such as N-bromocaprolactone amine to make it aromatize, the reaction time is long and the cost is high. West G...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/84C07C67/333C07C67/307C07C69/757
CPCC07C67/307C07C67/333C07C2601/14C07C69/757C07C69/84
Inventor 李军高志国魏小纪
Owner 兰州馥尔盛科技发展有限公司