Galaxolide green synthesis technology

A green synthesis technology of Jiale musk, applied in chemical recycling, organic chemistry, etc., can solve the problems of high cost, difficult waste liquid treatment, high toxicity of chlorobenzene, etc., to increase production rate, improve equipment corrosion and harm to staff Physical damage, reduce the effect of "three wastes" pollution

Inactive Publication Date: 2018-09-28
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] Current reports have the disadvantages of low yield, difficult waste liquid treatment, and high cost in the green synthesis technology 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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  • Galaxolide green synthesis technology

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Experimental program
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Effect test

Embodiment 1

[0029] Sulfonic acid type strongly acidic cation exchange resin, its preparation method comprises the following steps,

[0030] (1) Put 0.25g of gelatin into a four-necked flask equipped with 60.0g of deionized water, stir and heat up to 45°C, add 0.025g of hydroxymethylcellulose after the gelatin is dissolved, and use 5% NaOH aqueous solution and 5% boric acid Aqueous solution The pH of the aqueous phase was adjusted to 10 to obtain a hydrosol solution. 0.5 g of dibenzoyl peroxide was added to 18 g of glycidyl methacrylate and 8.7 g of divinylbenzene mixture, and added to the above-mentioned hydrosol solution for suspension polymerization to obtain 53 g of bead-shaped cross-linked copolymer skeletons.

[0031] (2) 10 g of the bead-shaped cross-linked copolymer skeleton obtained in step (1) is added to 50 mL of 15% sodium sulfamate aqueous solution and 30 g of N, N-dimethylmethylene formamide at a pH of 8 The sulfonic acid type strongly acidic cation exchange resin is obtaine...

Embodiment 2

[0033] Sulfonic acid type strongly acidic cation exchange resin, its preparation method comprises the following steps,

[0034] (1) Put 0.35g of gelatin into a four-necked flask equipped with 60.0g of deionized water, stir and heat up to 45°C, add 0.025g of hydroxymethylcellulose after the gelatin is dissolved, and use 5% NaOH aqueous solution and 5% boric acid Aqueous solution The pH of the aqueous phase was adjusted to 11 to obtain a hydrosol solution. 0.8 g of dibenzoyl peroxide was added to 20.0 g of glycidyl methacrylate and 12 g of divinylbenzene mixture, and added to the above-mentioned hydrosol solution for suspension polymerization to obtain 25 g of bead-shaped cross-linked copolymer skeletons.

[0035] (2) 15 g of the bead-shaped cross-linked copolymer skeleton obtained in step (1) is added to 60 mL of 17% sodium sulfamate aqueous solution and 42 g of N,N-dimethylmethylene formamide at a pH of 8 The sulfonic acid type strongly acidic cation exchange resin is obtaine...

Embodiment 3

[0037] (1) Synthesis of pentamethylindane

[0038]Add tert-amyl alcohol 88g and 5.6g of sulfonic acid type strongly acidic cation exchange resin prepared in Example 1 into the reactor, then add α-methylstyrene 100g dropwise to the reactor while stirring; control the stirring speed and the dropping speed , reacted at 40°C for 10 hours. The reacted material was left to stand, layered, filtered to separate the sulfonic acid type strongly acidic cation exchange resin catalyst for reuse, and the organic phase was rectified to separate the unreacted raw material to obtain 123.2 g of indane, with a yield of 72.8%;

[0039] (2) Synthesis of hexamethylindanol

[0040] Add 18.8g of pentamethylindane and 100mL of dichloromethane into the reactor, and add anhydrous 1.3g of ZnCl at a temperature of -15°C 2 , and turn on the stirrer, after stirring for a period of time, slowly add 29g of propylene oxide in 30mL of dichloromethane solution, continue to react for 10 hours, add to the ice-wa...

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Abstract

The invention relates to a galaxolide green synthesis technology. During preparation of an intermediate pentamethyl indane, the prepared sulfonic acid-type strong-acid cation exchange resin is selected as a catalyst for a reaction under solvent-free condition, three wastes pollution is reduced, solid catalysis is easy for separation, the technology is in favor of industrial production, and the yield can achieve as high as more than 70%.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a green synthesis process of carole musk. Background technique [0002] Natural musk source is few, is difficult for obtaining, and every kilogram of musk needs the sachet of 60 male musk deer, and the annual output of natural musk in the whole world is about 350k (content 70%) at present. With the imbalance of ecological balance, the resources of natural musk are becoming increasingly scarce. Due to the deterioration of the ecological environment and excessive hunting, the resources of wild musk deer in my country have shrunk sharply, and the existing number is less than 1 / 10 of that in the middle of the 20th century. For this reason, in the 1980s, the musk deer in my country was listed as a national first-class protected animal, and any form of hunting was strictly prohibited. People have tried to obtain musk by artificially raising musk deer and extracting incense f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/94
CPCC07D311/94Y02P20/584
Inventor 董秋月
Owner 杭州更蓝生物科技有限公司
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