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Synthetic process of galaxolide

A technology of Jiale musk and synthesis process, applied in the direction of organic chemistry, can solve the problems of difficult waste liquid treatment, high cost, high toxicity of chlorobenzene, etc., and achieve the effects of reducing the pollution of "three wastes", increasing production rate, and improving equipment corrosion

Inactive Publication Date: 2018-07-06
杭州更蓝生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process uses acetic acid as a catalyst in the process of preparing indan, and the waste liquid is difficult to deal with, seriously polluted, and the yield is 48%. In the process of preparing indanol, excessive pentamethylindane needs to be used as raw material and solvent, and the cost is relatively high , productive rate is lower only 48%; Also useful chlorobenzene is made solvent, productive rate 58.4%, but the toxicity of chlorobenzene is big, influences the application scope of product; The reaction produces highly toxic by-product chloromethyl ether with a yield of 90%.
[0008] At present, it is reported that there are low yields, difficult waste liquid treatment, high cost and other shortcomings in the synthesis process of Jiale musk. The present invention aims at the deficiencies of the prior art, improves the existing process by selecting better catalysts and solvents, and reduces " "Three wastes" pollution and equipment corrosion problems, while improving yield and reducing costs

Method used

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  • Synthetic process of galaxolide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation method of the macroporous strong acid styrene cation exchange resin includes the following steps:

[0029] 1) Prepare solution A with 300 mL of 0.5% polyvinyl alcohol and 400 mL of ammonium sulfate solvent with a mass concentration of 4%;

[0030] 2) Take 10g of chloropropylene oxide, 20g of polyethylene polyamine and 200mL of toluene to prepare solution B;

[0031] 3) Resin preparation: increase the temperature of solution A to 30°C, add solution B while stirring, stir well and increase the temperature to 90°C, polymerize for 3 hours, then soak the obtained resin in ether for 5-6 hours, and then clean water Carry out multiple cleanings and vacuum drying, the drying temperature is 60~80℃, and the vacuum degree is 100Pa.

Embodiment 2

[0033] The preparation method of the macroporous strong acid styrene cation exchange resin includes the following steps:

[0034] 1) Prepare solution A with 0.8% polyvinyl alcohol and 4.5% ammonium sulfate solvent;

[0035] 2) Take 5 g of chloropropylene oxide, 20 g of polyvinyl polyamine and 30 mL of xylene to prepare solution B;

[0036] 3) Resin preparation: The solution A was heated to 40°C, and solution B was added while stirring. After thorough stirring, the temperature was raised to 100°C, and the polymerization reaction was carried out for 4 hours. Then the obtained resin was soaked in ether for 5 hours, and then cleaned with water. The second cleaning, vacuum drying, the drying temperature is 80 ℃, the vacuum degree is 100 Pa.

Embodiment 3

[0038] (1) Synthesis of pentamethylindan

[0039] Add 88 g of tert-amyl alcohol and 8.8 g of the macroporous strongly acidic styrene cation exchange resin prepared in Example 1 into the reactor, and then add 100 g of α-methyl styrene to the reactor while stirring; control the stirring speed and Dropping rate, react at 40°C for 10 hours. The reacted materials are left to stand, layered, filtered to separate the macroporous strong acid styrene cation exchange resin catalyst, which can be reused, and the organic phase is rectified to separate the unreacted raw materials to obtain 121.8 g of indane, with a yield of 72%;

[0040] (2) Synthesis of hexamethylindanol

[0041] Add 18.8g of pentamethylindane and 100mL of dichloromethane into the reactor, and add anhydrous 1.3g of AlCl at a temperature of -15°C 3 , And turn on the stirrer, slowly add 29 g of propylene oxide in 30 mL of dichloromethane solution after stirring for a period of time, continue the reaction for 10 hours, add to the ...

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Abstract

The invention relates to a synthetic process of galaxolide. When an intermediate 1,1,2,3,3-pentamethylindane is prepared, macroporous strong-acidic styrenes cation exchanging resin prepared by the process is selected as a catalyst to react under a condition of no solvent, so that the pollution of waste gas, waste solids and waste water can be reduced, the solid catalysis is easy to separate, the industrialized production is facilitated, and the yield reaches up to 70 percent or more.

Description

Technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a synthesis process of Jiale Musk. Background technique [0002] Natural musk has few sources and is not easy to obtain. Each kilogram of musk requires 60 male musk deer sachets. At present, the annual output of natural musk in the world is about 350k (70% content). With the imbalance of ecological balance, natural musk resources are increasingly scarce. Due to the deterioration of the ecological environment and excessive hunting, the amount of wild musk deer in my country has shrunk sharply, and the current amount is less than 1 / 10 of that in the middle of the 20th century. For this reason, in the 1980s, musk deer in our country was listed as a national first-class protected animal, and hunting in any form was strictly prohibited. People have tried to obtain musk by artificially raising musk deer and extracting incense from living bodies. Due to the irritable nature of mal...

Claims

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Application Information

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IPC IPC(8): C07D311/94
CPCC07D311/94
Inventor 董秋月
Owner 杭州更蓝生物科技有限公司
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