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Method for preparing oxabicyclohexadecene

An oxabicyclo and hexadecene technology is applied in the field of preparation of oxabicyclohexadecene, and can solve the problems of large amount of waste water, low nucleophilic substitution reaction yield, difficulty in purification and post-treatment, and the like, and achieves low cost of raw materials , the process route is simple, the effect of less by-products

Active Publication Date: 2021-01-22
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the nucleophilic substitution reaction yield of this reaction is too low, the amount of waste water is large, the purification and post-treatment are difficult; the free radical addition reaction is not easy to control, the post-treatment system emulsifies seriously, and high polymers will be generated in industry

Method used

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  • Method for preparing oxabicyclohexadecene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Preparation of supported organometallic catalysts:

[0036] Mix 200.75g of rhodium acetate and 204.01g of 2,6-bisdiphenylphosphinopyridine in 800g of distilled water, raise the temperature to 60°C and stir for 4 hours; add 178.59g of 4A molecular sieve under stirring to obtain a slurry;

[0037] Use 25wt% sodium bicarbonate solution as the alkaline precipitant, heat the slurry and the alkaline precipitant to 50°C respectively, and slowly add the alkaline precipitant to the slurry until the pH of the system is 10.0, and control the reaction temperature of the precipitation process 50°C; After the precipitation reaction is completed, the slurry is obtained after aging at 70°C for 6 hours;

[0038] Then the slurry was fully filtered, the surface of the filter cake was washed with deionized water, and the filter cake was dried at 90°C for 9 hours to obtain the dried filter cake, which was then calcined at 190°C for 6 hours, crushed and pressed into tablets to obtain the cat...

Embodiment 2

[0042] Preparation of supported organometallic catalysts:

[0043] Mix 311.27g of rhodium chloride and 255.13g of 1-(2-diphenylphosphine-1-naphthalene)isoquinoline in 800g of distilled water, raise the temperature to 60°C and stir for 4 hours; add 102.05g of 4A molecular sieve under stirring to obtain a slurry ;

[0044] Use 25wt% sodium bicarbonate solution as the alkaline precipitant, heat the slurry and the alkaline precipitant to 50°C respectively, and slowly add the alkaline precipitant to the slurry until the pH of the system is 10.0, and control the reaction temperature of the precipitation process 50°C; After the precipitation reaction is completed, the slurry is obtained after aging at 70°C for 6 hours;

[0045] Then the slurry was fully filtered, the surface of the filter cake was washed with deionized water, and the filter cake was dried at 90°C for 9 hours to obtain the dried filter cake, which was then calcined at 190°C for 6 hours, crushed and pressed into table...

Embodiment 3

[0050] Preparation of supported organometallic catalysts:

[0051] Mix 300.9g of rhodium chloride and 209.2g of 2-(diphenylphosphine)methylpyrrolidine in 800g of distilled water, raise the temperature to 60°C and stir for 4 hours; add 153.07g of ordered mesoporous carbon under stirring to obtain a slurry;

[0052] Use 25wt% ammonium carbonate solution as an alkaline precipitant, heat the slurry and the alkaline precipitant to 50°C, and slowly add the alkaline precipitant to the slurry until the pH of the system is 11.0, and control the reaction temperature of the precipitation process to 50°C °C; After the precipitation reaction is completed, the slurry is obtained after aging at 70 °C for 6 hours;

[0053] Then the slurry was fully filtered, the surface of the filter cake was washed with deionized water, and the filter cake was dried at 100°C for 10 hours to obtain the dried filter cake, which was then calcined at 180°C for 8 hours, crushed and pressed into tablets to obtain th...

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Abstract

The invention discloses a method for synthesizing an important intermediate oxabicyclohexadecene of cyclopentadecanolide by a one-step method. Cyclododecene and acrolein are subjected to a cycloaddition reaction under the action of a supported metal organic catalyst to obtain an intermediate oxabicyclo hexadecene of the cyclopentadecanolide, wherein the supported metal organic catalyst is represented as Rh-X / Y, wherein X is one or more of 2 -(diphenylphosphine) methyl pyrrolidine, 2, 6-bis (diphenylphosphino) pyridine and 1-(-2-diphenylphosphine-1-naphthalene) isoquinoline, Y is a carrier andis selected from one or more of 4A molecular sieves, ordered mesoporous carbon, neutral aluminum oxide and silicon dioxide.

Description

technical field [0001] The invention relates to a preparation method of oxabicyclohexadecene. [0002] technical background [0003] Musk is a rare animal spice with a very special and delicate aroma. It is also widely used in society, such as: daily chemical, food, tobacco, pharmaceutical and other industrial industries. Because the musk fragrance market demand is large, and natural musk can not meet market demand far away, so people begin to supplement part of the industrial demand with synthetic musk. Synthetic musks on the market are mainly divided into nitro musks, polycyclic musks, and macrocyclic musks. Among them, nitro musk has been basically withdrawn from the market due to the shortcomings of accumulation in the human body, photosensitivity, and carcinogenicity; although the technology of polycyclic musk is mature, recent studies have found that polycyclic musk cannot be biodegraded, which will cause accumulation in the food chain. , there are potential safety ha...

Claims

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Application Information

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IPC IPC(8): C07D311/94B01J31/24
CPCC07D311/94B01J31/2404B01J31/2447B01J2531/822B01J2531/0238B01J2231/326
Inventor 李建锋陈来中刘杰张永振郭斌潘亚男
Owner WANHUA CHEM GRP CO LTD
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