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Process for preparing benorilate amyl alcohol

A preparation process, the technology of phenphenoperol, which is applied in hydrogenation preparation, organic chemistry, etc., can solve the problems of high cost, difficult cost reduction, and unsatisfactory selectivity, and achieve high yield, high hydrogenation yield, and promotion value high effect

Inactive Publication Date: 2015-09-02
江苏绿源精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Due to the easy poisoning and high price of the palladium-carbon catalyst, it is difficult to reduce the cost of the product; as a non-precious metal catalyst, the nickel catalyst has the advantage of low price, and at the same time, the tolerance to impurities in the starting material is much higher than that of the palladium-carbon catalyst , but the activity of the nickel catalyst to reduce the dihydrofuran ring is low, and the selectivity is not ideal

Method used

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  • Process for preparing benorilate amyl alcohol
  • Process for preparing benorilate amyl alcohol
  • Process for preparing benorilate amyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step A: Take one 2000mL four-necked flask as a reaction kettle, add 400g of benzaldehyde, 400g of tert-butylbenzene, and 1g of iron sulfate. Turn on the stirring, raise the temperature of the materials in the kettle and control the reaction temperature to 150-155°C, add 350g of prenyl alcohol to the reaction kettle dropwise through the dropping funnel, as the addition proceeds, the reaction will produce water, and the produced water will be separated by a water separator. The water is removed, and the steamed upper oil phase is returned to the reactor.

[0030] Step B: After the dropwise addition, continue to reflux to separate the water. When the water is divided to 67mL, stop the water separation, drop to 50°C, and wash with water. The pH of the water washing must be greater than 6. After the pH is qualified, remove the water to obtain 1070g of the oil phase. The oil phase was rectified under reduced pressure to obtain 602 g of phenyldihydropyran with a content of 96%...

Embodiment 2

[0035] Repeat the steps A to B above to recover 604g of phenyldihydropyran with a content of 95% and recover 505g of tert-butylbenzene. The recovered tert-butylbenzene contains a small amount of benzaldehyde and prenol.

[0036] Step C: Put 604g of recovered phenyldihydropyran, 14g of recovered Raney nickel and newly added 3g of Raney nickel into a 1000mL hydrogenation kettle to raise the temperature to 130-140°C, pressure 0.6-1MPa, and start hydrogenation , after hydrogenation to 3mol, the reaction time is 2.5h, the hydrogenation is about 40% of the theoretical hydrogenation amount, stop hydrogenation, cool down, and filter.

[0037] Step D: Put the hydrogenation filtered clear liquid back into the hydrogenation kettle, put in the first batch of recycled palladium carbon and 1g of new 5% palladium carbon, and heat up to 130-140°C, pressure 0.5-0.6MPa, and start hydrogenation. The hydrogenation continued for 4.5 hours until no more hydrogen was absorbed, the reaction was stopp...

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Abstract

The invention belongs to the technical field of fine chemicals and relates to benorilate amyl alcohol, particularly a process for preparing benorilate amyl alcohol. According to the technical scheme of the invention, phenyl dihydro pyran is synthesized firstly, and then is hydrogenated preliminarily. The reaction liquid of phenyl dihydro pyran is filtered, and the filtered clear liquid is hydrogenated. After that, the filtered clear liquid is filtered and washed, and benorilate amyl alcohol can be obtained through decompressing and rectifying the obtained crude product. According to the invention, benorilate amyl alcohol is prepared by means of a Raney-Ni catalyst and a Pd / C catalyst successively through the secondary hydrogenation process, so that the hydrogenation yield is high. Meanwhile, enorilate amyl alcohol, as a final product, is large in yield. Therefore, the industrialization of the above process is high in production and promotion value.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to phenphenoperol, in particular to a preparation process of phenphenoperol. Background technique [0002] Phenopentanol, the chemical name is 3-methyl-5-phenyl-pentanol, also known as phenylisohexanol, and its structural formula is: It is a commonly used rose fragrance series spice. Due to its extraordinary fragrance persistence and natural rose absolute floral fragrance, it is widely used in high-end daily fragrance, personal care and home care products. [0003] Swiss patent (patent No.: 6559323) has reported a kind of synthetic method of phenylpentanol, and raw material is that benzaldehyde and isoprene glycol are polymerized to produce phenyl dihydropyran under acidic conditions, then add under palladium carbon catalyst. Hydrogen makes 3-methyl-5-phenyl-pentanol, and its reaction equation is as follows: [0004] [0005] The iFF patent (CN102731260A) reports the syn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/20C07C29/17
CPCC07C29/17C07D309/18C07C33/20
Inventor 范忠辉陈晓龙林广德李安
Owner 江苏绿源精细化工有限公司
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