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Synthesis method of musk ambrette

A synthesis method and technology of musk sunflower, applied in the field of essence, can solve the problems of low production efficiency and large amount of waste water, and achieve the effects of reducing energy consumption and saving human resources

Inactive Publication Date: 2017-12-01
TIANJIN ANKAITE CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The synthesis of m-cresol methyl ether in the traditional process adds phase transfer catalyst in sodium hydroxide aqueous solution, drops dimethyl sulfate and m-cresol mixed solution to generate (large amount of waste water, low production efficiency), and then m-cresol methyl ether In the presence of sulfuric acid, it is prepared by alkylating isobutanol to tert-butylmethoxytoluene, and finally nitrating it with nitric acid

Method used

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  • Synthesis method of musk ambrette
  • Synthesis method of musk ambrette

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The synthetic method of described sunflower musk, comprises the steps:

[0029] (1) Add 108g (0.99mol, 99%) m-cresol, 355g20% sodium hydroxide (1.775mol) aqueous solution, 4.3g (0.023mol, 99%) benzyltrimethylammonium chloride in 1000ml autoclave , 60.5g (1.186mol, 99%) methyl chloride carries out methoxylation reaction, is warming up to 80 ℃, is incubated 6-8 hour, sampling analysis selectivity 96.2%, then separates organic phase and neutralizes with 35% hydrochloric acid, after After washing and rectification under reduced pressure, 113.3 g of m-methylanisole was obtained, with a content of 98.5%, and a molar yield of 91.6%. The reason for affecting the yield was that the high concentration of sodium hydroxide formed a side reaction polymer;

[0030] (2) In four bottles of 1000ml equipped with reflux condenser, constant pressure dropping funnel, and chlorine trap, add 122g (1.42mol, 99%) of methylene chloride, 56g (0.41mol, 98%) of anhydrous aluminum trichloride %), t...

Embodiment 2

[0033] The synthetic method of described sunflower musk, comprises the steps:

[0034] (1) in 1000ml autoclave, add 108g (0.99mol, 99%) m-cresol, 355g15% (1.33mol) sodium hydroxide aqueous solution, 4.3g (0.023mol, 99%) benzyl trimethyl ammonium chloride, 60.5g (1.186mol, 99%) methyl chloride, warming up to 100°C and insulated for 6-8 hours to carry out methoxylation reaction, sampling analysis selectivity 97.1%, then separate the organic phase and neutralize with 35% hydrochloric acid, after washing, After rectification under reduced pressure, 112.5 g of m-methylanisole was obtained, with a content of 98.3% and a molar yield of 90.8%. The main reason for affecting the yield was that the high temperature formed side reaction polymerization;

[0035] (2) In four bottles of 1000ml equipped with a reflux condenser, a constant pressure dropping funnel, and a chlorine trap, add 122g (1.42mol, 99%) of methylene chloride, 41g (0.3mol, 98%) of anhydrous aluminum trichloride %), contr...

Embodiment 3

[0038] The synthetic method of described sunflower musk, comprises the steps:

[0039](1) in 1000ml autoclave, add 108g (0.99mol, 99%) m-cresol, 355g15% sodium hydroxide (1.33mol) aqueous solution, 4.3g (0.023mol, 99%) benzyl trimethyl ammonium chloride, 60.5g (1.186mol, 99%) of methyl chloride was heated to 70°C and kept for 6-8 hours, and the selectivity of sampling analysis was 94.8%, then the organic phase was separated and neutralized with 35% hydrochloric acid, washed and rectified under reduced pressure to obtain m-methylanisole 113.5g, content 99%, molar yield 92.2%, the main reason for affecting the yield is the incomplete reaction of raw material m-cresol at low temperature;

[0040] (2) In four bottles of 1000ml equipped with a reflux condenser, a constant pressure dropping funnel, and a chlorine trap, add 122g (1.42mol, 99%) of methylene chloride, 34g (0.025mol, 98%) of anhydrous aluminum trichloride %), control the temperature in the bottle at 0-5°C and add 123.2...

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Abstract

The invention provides a synthesis method of musk ambrette. The synthesis method comprises the following steps of (1) mixing m-cresol, a phase transfer catalyst, a water solution of strong alkali and chloromethane, reacting and then generating m-methoxytoluene; and (2) mixing a catalyst and a solvent, dropwise adding the m-methoxytoluene for 0.5-2h, dropwise adding tert-butyl chloride for 0.5-2h, then reacting for 3-5h and generating tertiary butyl methoxyl methylbenzene. According to the synthesis method of the musk ambrette, methylanisole (replenishing sodium hydroxide to an aqueous alkaline solution, filtering out sodium chloride and then recycling) is synthesized by m-cresol and chloromethane in the water solution of strong alkali, so that compared with a traditional production technology, the yield is improved, treatment of waste water is reduced, manpower resource is saved, energy consumption is reduced and the synthesis method is safer and more reliable.

Description

Technical field [0001] The invention belongs to the field of flavors, and in particular relates to a method for synthesizing sunflower musk. Background technique [0002] Sunflower musk is used in the preparation of many fragrances and as a fixative. Artificial musk is one of the best-smelling nitro-containing artificial musks. One of the commonly used nitro musks, suitable for various daily fragrances. [0003] The synthesis of m-cresol methyl ether in the traditional process involves adding a phase transfer catalyst to the sodium hydroxide aqueous solution, and adding a mixture of dimethyl sulfate and m-cresol dropwise to generate it (large amount of waste water, low production efficiency), and then m-cresol methyl ether is regenerated. In the presence of sulfuric acid, it is hydrocarbonated with isobutanol to tert-butylmethoxytoluene, and finally nitrated with nitric acid. Contents of the invention [0004] In view of this, the present invention aims to propose a syn...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/37
CPCC07C201/08C07C41/16C07C41/30C07C205/37C07C43/205
Inventor 潘建民高志国王增端陈鹏
Owner TIANJIN ANKAITE CATALYST
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